Note: Descriptions are shown in the official language in which they were submitted.
1338179
CANINE BISCUITS
CONTAINING AN INORGANIC PYROPHOSPHATE
BROAD DESCRIPTION OF THE INVENTION
An ob~ect of the lnventlon ls to provlde dry animal
biscuits containing pyrophosphate, partlcularly dog blscuits
contalnlng pyrophosphate. Another obiect of the lnventlon ls
to provlde a process for preparlng dog blscults contalning
pyrophosphate. Another ob~ect of the invention is to provide
a process for the prevention of tartar accumulation on the
teeth of dogs. A further ob~ect of the invention is to pro-
vide a process for the prevention of tartar accumulation on
the teeth of dogs by the chewing and eating of dog biscuits
contalning pyrophosphate by the dogs.
An ob~ect of the invention is to provide
nutritionally-balanced dry biscuits contalnlng pyrophosphate.
Another ob~ect of the invention is to provide a process for
preparing nutritionally-balanced dog biscults containing pyro-
phosphate. Another ob~ect of the inventlon is to provide a
process for the prevention of tartar accumulation on the teeth
of dogs. A further ob~ect of the inventlon ls to provlde a
process for the prevention of tartar accumulation on the teeth
of dogs by the chewlng and eating of nutrltlonally-balanced
dog biscuits contalning pyrophosphate by the dogs.
An ob~ect of the lnvention is to provlde dog blscuits
having a coating contalnlng at least one pyrophosphate.
Another ob~ect of the lnventlon ls to provlde a process for
preparlng dog blscults, havlng a coatlng containing at least
one pyrophosphate. Another ob~ect of the lnventlon ls to
a~
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1338179
provlde a process for the preventlon of tartar accumulatlon on
the teeth of dogs. A further ob~ect of the lnvention ls to
provide a process for the preventlon of tartar accumulation on
the teeth of dogs by the chewlng and eatlng of dog blscults
having a coatlng containlng at least one pyrophosphate by the
dogs.
An ob~ect of the lnventlon ls to provlde raw hlde
contalnlng pyrophosphate, partlcularly ln strlp form. Another
ob~ect of the lnventlon ls to provlde a process for preparlng
raw hlde, partlcularly ln strip form, contalnlng pyrophos-
phate. Another ob~ect of the lnventlon ls to provlde a process
for the preventlon of tartar accumulatlon on the teeth of
dogs. A further object of the lnventlon ls to provlde a pro-
cess for the preventlon of tartar accumulatlon on the teeth of
dogs by the chewlng and eatlng of raw hlde contalnlng pyro-
phosphate, partlcularly ln strlp form, by the dogs.
An ob~ect of the lnvention ls to provlde raw hlde
havlng a coatlng contalnlng pyrophosphate, partlcularly ln
strlp form. Another ob~ect of the lnventlon ls to provlde a
process for preparlng raw hlde, partlcularly ln strlp form,
havlng a coatlng contalnlng pyrophosphate. Another ob~ect of
the inventlon ls to provlde a process for the preventlon of
tartar accumulatlon on the teeth of dogs. A further ob~ect of
the lnventlon ls to provide a process for the preventlon of
tartar accumulatlon on the teeth of dogs by the chewlng and
eatlng of raw hlde, partlcularly ln strlp form, havlng a
coatlng containlng pyrophosphate by the dogs. Another ob~ect
ls to provlde a coatlng for human or animal baked dough prod-
ucts.
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1338173
An object of the invention is to provide devices,
compositions and the like containing pyrophosphate. A further
object of the invention is to provide processes for the
prevention or reduction of tartar accumulation on the teeth of
dogs by such devices, compositions and the like. Other
objects and advantages of the invention are set out herein or
are obvious herefrom to one skilled in the art.
The objects and advantages of the invention are achieved
by the compositions, processes, devices, etc., of the
invention.
The invention involves a process for preparing dog
biscuit dough which contains at least one inorganic
pyrophosphate. The process includes admixing the ingredients
of the biscuit dough and the at least one inorganic
pyrophosphate. The inorganic pyrophosphate also reduces the
accumulation of tartar on the teeth of dogs.
Tartar is an incrustation of the teeth consisting of
salivary secretion, food residue and various salts, such as,
calcium carbonate or phosphate. Tartar is also termed dental
calculus.
Caries are cavities or decay of the teeth which begins at
the surface of the tooth and may progress through the dentine
into the pulp cavity. It is believed that the action of
microorganisms in the mouth on ingested sugars and
carbohydrates produces acids that eat away the enamel. By
preventing the formation of calculus or tartar, the invention
formulation is in effect an anti-cariogenic agent.
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73783-60
This invention relates to baked dog food comprising a
soft center portion and an outer portion, the center portion
comprising at least one alkali metal inorganic pyrophosphate, the
center portion being softer than the outer portion, the center
portion containing about 0.1 to about 10 weight percent of said at
least one alkali metal inorganic pyrophosphate, based upon the
total weight of the baked dog food, said at least one alkali metal
inorganic pyrophosphate being water soluble, the baked dog food
being slightly acidic to neutral, the baked dog food having a
water activity of 0.70 or less, and the baked dog food containing
15 weight percent or less, based upon the total weight of the
baked dog food, of water.
This invention further provides a process for making a
baked blscuit for the prevention of tartar accumulation on the
teeth of a dog or a cat, by chewing or eating by the dog or cat of
a tartar inhibiting amount of at least one baked dog biscuit or
baked cat biscuit, respectively, the process comprising forming a
dough by admixing ingredients comprising flour, water, and an
effective antitartar amount of at least one alkali metal inorganic
pyrophosphate, the amount of said at least one alkali metal
inorganic pyrophosphate being sufficient to deliver from about 0.5
to about 3.5 weight percent, based on the total weight of the at
least one baked dog biscuit or baked cat biscuit containing at
least one alkali metal inorganic pyrophosphate, of P2O7, said at
least one alkali metal pyrophosphate being water soluble, forming
the dough into pieces, and baking the pieces, the at least one
baked dog biscuit or baked cat biscuit containing at least one
1338179
73783-60
alkali metal inorganic pyrophosphate being slightly acid to near
neutral, the at least one baked dog biscuit or baked cat biscuit
having a water activity of 0.70 or less, and the at least one
baked dog biscuit or baked cat biscuit containing about 5 to about
15 weight percent, based on the total weight of the at least one
baked dog biscuit or baked cat biscuit, of water.
The invention also relates to a process for making raw
hide for the prevention of tartar accumulation on the teeth of a
dog, by chewing or eating by the dog of a tartar inhibiting amount
of raw hide, the process comprising coating raw hide with an
edible coating comprising an effective antitartar amount of at
least one alkali metal inorganic pyrophosphate, the amount of said
at least one alkali metal inorganic pyrophosphate being sufficient
to deliver from about 0.1 to about 5 weight percent, based on the
total weight of the raw hide containing at least one alkali metal
inorganic pyrophosphate, of P207, said at least one alkali metal
inorganic pyrophosphate being water soluble, and drying the
coating, the raw hide containing an edible coating containing at
least one alkali metal inorganic pyrophosphate being slightly acid
to near neutral, and the raw hide containing an edible coating
containing at least one alkali metal inorganic pyrophosphate being
chewable, tough and flexible.
The invention also provides a process for making pet
foods for the prevention of tartar accumulation on the teeth of a
dentulous animal, by chewing or eating by the animal of a tartar
inhibiting amount of animal food, the process comprlsing coating
an animal food with an effective antitartar amount of at least one
3b
13~8179
73783-60
alkali metal inorganic pyrophosphate, the amount of said at least
one alkali metal inorganic pyrophosphate being sufficient to
deliver from about 0.1 to about 5 weight percent, based on the
total weight of the animal food containing at least one alkali
metal inorganic pyrophosphate, of P2O7, said at least one alkali
metal inorganic pyrophosphate being water soluble.
As well, the invention provides a baked dog or cat
biscuit which comprises a tartar-reduction effective amount of at
least one metal inorganic phosphate of the formula Mn+2PnO3n+1,
wherein M is a univalent metal and n is 2, 3, 4 or 5, or of the
formula M'nPnO3n+1, where M' is a divalent metal and n has the
above meaning, said at least one metal phosphate having an oxide
ratio of cationic oxides (M2O or M'O) and anionic oxides (P205)
being between 1 and 2 or being 2.
1338179
Preferably the dry dough lngredients and the inor-
ganic pyrophosphate salts are mixed, then water is added and
the mixing continued, and finally the fat (tallow) is added
and thoroughly mixed in.
The dog biscuits can be made from any suitable dough.
In one advantageous embodiment, a bone-shaped canine biscuit
is provided which is baked from a dough comprising wheat
flour, wheat meal, soybean meal, meat and bone meals, animal
fat and water.
The dog biscuit dough preferably contalns about 0.1
to about 10 weight percent of the at least one lnorganlc
pyrophosphate compound, and most preferably about 0.5 to about
5 weight percent of said at least one inorganic pyrophosphate
compound. The preferred lnorganlc pyrophosphate salt(s) ls an
alkali metal pyrophosphate. While the preferred alkali metal
pyrophosphate is tetrasodium pyrophosphate, most preferably
the dog biscuit dough contains a combination of sodium acid
pyrophosphate and tetrapotassium pyrophosphate (or tetrasodium
pyrophosphate).
The invention also involves a process for preparing
unbaked dog biscuits from the dog biscuit dough. The inven-
tion also involves unbaked dog biscuits which contain at least
one inorganic pyrophosphate. The dog blscuit pieces preferab-
ly are bone shaped. The unbaked dog biscuits preferably have
a moisture content usually in the range of about 25 to about
40 weight percent, preferably about 33 to about 35 weight
percent.
D 73783-60
13~817g
The invention also involves a process for preparing baked
dog biscuits which contain at least one inorganic
pyrophosphate. The process includes:
(a) shaping a dog biscuit dough, which contains the at
least one inorganic pyrophosphate, into dog biscuit pieces
comprising unbaked dog biscuits; and
(b) baking the unbaked dog biscuits.
The baked dog biscuits can be dried, if necessary, to obtain
the desired moisture level. The baked dog biscuits should
have a moisture content of 13 weight percent or less,
advantageously between about 5 and 13 weight percent,
preferably between about 8 and about 12 weight percent.
The invention product is baked so that it comprises a
baked dog biscuit which contains at least one inorganic
pyrophosphate.
The invention further involves baked dog biscuits which
contain at least one inorganic pyrophosphate. The
ingredients, ratios, ranges, etc., for the invention dog
biscuit dough applies to the invention baked dog biscuits,
except as otherwise noted herein.
The invention product preferably should be slightly acid
to neutral.
The inorganic pyrophosphates are anti-tartar, anti-plaque
or anti-calculus agents. The invention product exhibits anti-
tartar properties over its normal shelf life. The invention
product does not adversely affect canine tooth enamel.
The invention further involves a process for the
prevention or reduction of tartar accumulation on the teeth of
133817~
dogs. The process lncludes the chewlng and/or eating of the
lnventlon baked dog blscults by the dogs. (The term "dog
biscult" hereln means a baked dog biscuit unless otherwlse
stated hereln or otherwise obvious herefrom to one skllled ln
the art.)
The lnventlon biscuits, when eaten and chewed by
dogs, cleans tooth surfaces, removes tartar (by mechanical
action~, and exercises and massages the gums. The pyrophos-
phate ln the lnvention blscuits prevents or reduces the forma-
tlon of tartar on the dog's teeth. The pyrophosphate, ln thelevels lnvolved, does not adversely affect the gastrolntestin-
al system or the health of the dogs.
As used hereln, all parts, percentages, ratlos and
proportlons are on a welght basis unless otherwlse stated
hereln or otherwlse obvious herefrom to one skilled in the
art. As used hereln, all temperatures are in degrees Fahren-
heit unless otherwlse stated hereln or otherwlse obvlous
herefrom to one skilled in the art.
Dental calculus, or tartar as it ls sometlmes called,
is a deposit which forms on the surfaces of the teeth at the
gingival margin. Supraglnglval calculus appears principally
ln the areas near the orifices of the salivary ducts; e.g., on
the llngual surfaces of the lower anterlor teeth and on the
buccal surfaces of the upper first and second molars, and on
the dlstal surfaces of the posterlor molars. Mature calculus
consists of an inorganic portion which is largely calclum
phosphate arranged ln a hydroxylapatlte crystal lattlce struc-
ture slmilar to one, enamel and dentine. An organic portion
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1338179
is also present and consists of desguamated epithelial cells,
leukocytes, salivary sediment, food debris and varlous types
of microorganlsms. As the mature calculus develops, it
becomes visibly whlte or yellowlsh in color unless stained or
discolored by some extraneous agency. In addition to being
unsightly and undesirable from an aesthetlc standpoint, the
mature calculus deposits are constant sources of irritatlon of
the ginglva and thereby are a contributlng factor to glngivl-
tls and other diseases of the supporting structures of the
teeth, the irrltation decreasing the reslstance of tlssues to
endogenous and exogenous organlsms.
The dog biscuits containing pyrophosphate can be made
from any suitable dough.
Any suitable dough comprising at least one flour,
meal, fat and water can be employed for the product. For
instance, when the desired product is a canine biscuit, a
conventional dough for dog biscults can be used, optionally
containlng discrete particles of meat and/or meat byproducts
or farinaceous material. Such doughs typically contain fat
solids. Examples of suitable doughs for the production of
hard dog biscuits are dlsclosed in U.S. Patent No. 4,454,163,
and suitable doughs for the production of soft dog biscuits
Icontaining humectant to control water activlty) are dlsclosed
ln U.S. Patent No. 4,454,164. Partlculate protelnaceous
particles, such as, particles of meat, texturized vegetable
protein and/or meat byproducts, can be lncorporated to add
flavor to the blscuits and texturize the surface. Particulate
farlnaceous materlals, such as, bran partlcles, can also be
-- 7 --
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13:~8179
employed to texturize the interior and/or surface of the
blscults and to provlde other useful propertles to the prod-
uct. A dough found to produce blscuits highly palatable to
dogs lncludes suitable proportlons of wheat flour, wheat meal,
soybean meal, meat and bone meal, anlmal fat and natural
flavors ln admlxture wlth water. The meal used ln the doughs
sultable for productlon of blscults useful ln the lnventlon
can comprlse meat and/or bone and/or vegetable matter lnclud-
lng farlnaceous materlals, materlals prepared from legumes
such as beans and peas, tuberous materlals such as potato
meal, and the llke. The meals can be flnely or coarsely
ground as deslred for the texture. Flours made from any
sultable farlnaceous materlal can be used.
The doughs generally have a water actlvlty of about
0.90 and above upon completion of mixing of the dough ingredl-
ents. A sultable dough contalns farlnaceous materlal, an
edlble oll, an antloxidant, an antimycotic, salt, animal fat,
added vltamlns and minerals, such as those dlsclosed ln U.S.
Patent No. 4,229,485, column 5, llnes 7 to 57. The composl-
tlons of the inventlon also preferably contaln at least oneanlmal-derlved protelnaceous meal such as meat meal, bone meal
and flsh meal. A good blscult dough for produclng the bls-
cults of the lnventlon contalns about 50 to 60 percent by
welght of wheat flour, about 5 to 10 percent by weight of
soybean meal, about 3 to 10 percent by welght of meat and bone
meal, about 1 to 5 percent
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of wheat meal, about 1 to 5 percent of animal fat preserved
with BHA, about 20 to 30 percent by weight of water, and about
2 to 5 percent by weight of natural flavors, vitamin and
mineral preblend, and acidulant.
The solvent used in preparing the dog biscuit dough, or
for incorporating certain ingredients therein, is most
preferably water, but other non-toxic, edible solvents, such
as, ethanol or ethanol/water, can be used. The problem of the
necessity of solvent removal from the dough due to toxicity is
to be avoided in most cases. If a mixture of ethanol and
water is used, the amount of ethanol in the mixture is
generally about 5 to about 60 percent, preferably about 5 to
about 25 percent. When one or more of the inorganic
pyrophosphates is not water soluble, it may be ethanol
soluble. It may be necessary to use a non-aqueous solvent, or
mixture of water therewith, to incorporate the inorganic
pyrophosphate.
The invention includes the use of at least one inorganic
pyrophosphate. Preferably the inorganic pyrophosphates are
water soluble or preferably a mixture of water soluble and
water insoluble inorganic pyrophosphates are used. Such a
mixture is usually used to provide a desired pH. The use of
water-insoluble or difficultly soluble inorganic
pyrophosphates in a dog biscuit dough is not a significant
problem compared to use of such materials in a solution, such
as, a mouth wash.
The pH of the dough can be adjusted using an inorganic
base (e.g., KOH, NaOH, CaOH, LioH~ MgOH, etc.) or an inorganic
13~8179
acld (e.g., H2SO4, HCl, etc.), but this approach has the
disadvantages of posslbly causlng a mlsbalance or
overabundance of one or more chemlcal entities and possibly
introduclng unwanted salts.
Generally 0.1 to 10 weight percent, advantageously
about 0.5 to about 5 weight percent, of inorganic pyrophos-
phate is used.
When a mixture of tetrasodium pyrophosphate (TSPP)
and sodium acld pyrophosphate ln aqueous solutlon at the 5
weight percent level was incorporated in dog biscuit dough,
there was reduced dough gluten development; the dog biscuits
were bleached (whltish) and crumbly; and the dog biscuits were
softer (a hardness problem) than the control dog biscuits. At
the level of 3 weight percent of a mixture of tetrasodium
pyrophosphate and sodium acid pyrophosphate, the same problems
occurred, but less severely. The addition of the lnorganlc
pyrophosphates ln dry form to the dry lngredients in the dough
preparation basically eliminated the above problems. It was
also found that better results were secured by using the
inorganlc phosphates ln powder form as opposed to granular
form.
The inorganic pyrophosphates are preferably alkali
metal pyrophosphates. The preferred alkall metal pyrophos-
phates are tetrasodium pyrophosphate and tetropotassium pyro-
phosphate. An example of a useful tetraalkall metal pyrophos-
phate is tetralithium pyrophosphate. Alkaline earth metal
pyrophosphates are also useful, but they are generally
-- 10 -
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1338179
insoluble in water. Preferably, the inorganic pyrophosphates
are soluble in water.
Kirk & Othmer, "Encyclopedia Of Chemical Technology", 2nd
Ed., Vol. 15, (1965), pages 232 to 276, discloses a number of
water-soluble inorganic pyrophosphate salts. The pertinent
portions of Kirk & Othmer, "Encyclopedia Of Chemical
Technology", 2nd Ed., Vol. 15, (1965), pages 232 to 276, are
incorporated herein by reference.
Examples of dialkaline metal pyrophosphates are dicalcium
pyrophosphate, dibarium pyrophosphate and dimagnesium
pyrophosphate. Trialkali metal monoacid pyrophosphates,~such
as, trisodium hydrogen pyrophosphate, can be used. Monoalkali
metal triacid pyrophosphates, such as, sodium trihydrogen
pyrophosphate, can also be present in limited amounts.
Examples of other inorganic pyrophosphates include manganese
pyrophosphate and dizinc pyrophosphate.
The formula Mn+2PnO3n+1~ where M is a univalent metal, is
the formula for univalent metal pyrophosphates when n is 2.
The formula M'nPnO3n+1, where M' is a divalent metal, is the
formula for divalent metal pyrophosphates when n is 2. Such
univalent metal pyrophosphates and divalent metal
pyrophosphates can be used in the invention. Polyphosphates
have the formula Mn+2PnO3n+, or M'nPnO3n+1, where n is 2, 3, 4, 5,
..., and the oxide ratio R between the cationic oxides (M20 or
M'O) and anionic oxides (P205) is between 1 and 2. The oxide
ratio for pyrophosphate is 2.
Tetrasodium pyrophosphate, one part, is soluble in 13
parts of cold water and in 2.5 parts of boiling water. It is
1338179
insoluble in ethanol. Dicalcium pyrophosphate is practically
insoluble in water. The invention use of the term "solution"
includes slurries, suspensions and the like. Tetrapotassium
pyrophosphate is freely soluble in water and is insoluble in
ethanol.
Advantageously a mixture of water-soluble tetrasodium
pyrophosphate or tetrapotassium pyrophosphate and water-
insoluble dicalcium pyrophosphate is used (in a ratio to
achieve the desired pH). Most preferably a mixture of sodium
acid pyrophosphate and tetrapotassium pyrophosphate is used
(in a ratio to achieve the desired pH). In such most
preferred mixture, tetrasodium pyrophosphate is not used as it
would provide too much sodium in the composition.
The maximum allowable GRAS level in a composition for
sodium acid pyrophosphate (SAPP) is 2.1 weight percent and
tetrapotassium pyrophosphate (TKPP) is 1.4 weight percent in
baked goods. If GRAS levels change (rise) or if higher levels
are allowed by the regulatory agencies, higher levels can be
used in the invention. TKPP delivers approximately 52.65
percent of P207; SAPP delivers about 78.36 percent of P207; and
TSPP delivers about 65.4 percent of P207.
~ The most preferred invention dough contains trisodium
monoacid pyrophosphate (that is, sodium acid pyrophosphate or
SAPP) and tetrapotassium pyrophosphate in a weight ratio of
about 60 to about 40.
The pyrophosphate(s) is used in sufficient amount to
deliver generally from about 0.1 to about 5, preferably from
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about 0.5 to about 3.5, most preferably 1.4 to 2.5 weight
percent (based on the total composition), of P207.
A study of the application of aqueous solutions of a
mixture of tetrasodium pyrophosphate and sodium acid
pyrophosphate to the teeth of dogs by spraying for one month
resulted in dose response data. The aqueous solutions
containing 5 and 3 weight percent of a mixture of tetrasodium
pyrophosphate and sodium acid pyrophosphate resulted in
significant reductions in tartar accumulation. The aqueous
solutions containing 1.5 and 0.5 weight percent of a mixture
of tetrasodium pyrophosphate and sodium acid pyrophosphate
resulted in directional trends of reductions in tartar
accumulation. See also U.S. Patent No. 3,323,551.
The ratio of sodium acid pyrophosphate (SAPP) to
tetrapotassium pyrophosphate (TKPP) is generally between 4 to
1 and 3 to 7, preferably between 7 to 3 and 1 to 1, most
preferably about 3 to about 2. SAPP has a pH of 4.2 and TKPP
(and TSPP) has a pH of 10.2, so the combination of SAPP and
TKPP (or TSPP) provides a resultant pH which is a balance of
the pHs of the two components.
The pH of the dough of at least one inorganic
pyrophosphate compound (salt) is generally in the range of
about 4 to about 10.5, typically from about 4.5 to about 7.5,
preferably from about 5 to about 7, most preferably between
about 5.6 and 6Ø Milk Bon ~ dog biscuit has a pH of 6.1 to
6.4. Tartar reduction is indicated to be best at neutral pH
and palatability is indicated to be best at a slightly acidic
133817~
pH, so the best mode contemplates a balance of such two
factors.
The dough ingredient is generally mixed at a temperature
of about 45 to about 140F, preferably about 60 to about
125F.
The dough can also contain suitable surfactants or
emulsifying agents, e.g., cationic agents and nonionic agents.
Suitable nonionic emulsifying agents can be broadly defined as
compounds produced by the condensation of alkylene oxide
groups (hydrophilic in nature) with an organic hydrophobic
compound which can be aliphatic, alkyl aromatic, or a
condensate of an alkylene oxide with an alkylene glycol in
nature. Examples of suitable nonionic emulsifying agents
include the Piuronics, polyethylene oxide condensates of alkyl
phenols, products derived from the condensation of ethylene
oxide with the reaction product of propylene oxide and
ethylene diamine, ethylene oxide condensates of aliphatic
alcohols, long chain tertiary amine oxides, long chain
tertiary phosphine oxides, long chain dialkyl sulphoxides, and
mixtures of such materials. The emulsifier is best used in
minor amounts.
~ The dog biscuit dough can be mixed using any suitable or
conventional equipment. For example, the mixing can be at 20
to 100 rpm. For example, a dry blending step (dries and the
inorganic pyrophosphates) can be done typically at room
temperature for a period of time of about 3 minutes to about
20 minutes. The dry-blended mixture can then be mixed with
the hot water to form a first stage dough. The water which
14
133~179
can be admixed with the dry-blended mixture is typically at a
temperature of about 65 to about 150F. The hot water can be
added, with mixing, over a period of time of about 3 minutes
to about 6 minutes to form the first stage dough. Then, the
fat portion of the biscuit dough can be admixed with the first
stage dough to form the final stage dough. The fat portion
can be added at a temperature at which it is at least fluid,
typically at about 100 to about 150F. The fat portion can be
mixed for a period of time which is sufficient to form a dough
whose homogeneity is visually apparent. A typically final
mixing time is about 3 to about 5 minutes.
If there are machinability and dough structure property
problems with the invention dough, the addition of water
should solve such problems. If the use of the higher water
levels causes the dough to be so sticky as to cause problems
in a sigma or rotary mixer (but normally not a significant
problem in a continuous mixer). The addition of more tallow
to the dog biscuit dough should assist in more effective
mixing and help to keep the dough from being so sticky that it
clings to the rotary molder. Preferably the tallow level is
about 2.6 to about 3.1 weight percent (most pr~ferably about
2.85 weight percent), as opposed to a tallow level of about
2Y46 weight percent in Milk Bone@~dog biscuits. Also, the
tallow provides a taste which dogs like.
Formation of the dough is achieved at about atmospheric
pressure with mixing of the components being conveniently
achieved in an upright sigma blade mixer or other bakery-type
mixers. The various ingredients can be added over a period of
- 133817~
time or in a one-shot manner according to the above order of
addition. However, melted fat and water can be added
simultaneously and mixed for 6 to 10 minutes.
The dog biscuits are formed in any conventional or
suitable manner, such as, by extrusion, stamping, cutting or
molding. Any suitable dog biscuit shapes can be used, such
as, a bone-shaped canine biscuit. For many products, such as,
the bone-shaped canine biscuits of the invention, a rotary
molding system is preferred because it permits the rapid
forming of dough pieces with good control over their shape,
form and surface characteristics. Docker holes are preferably
formed in the dough piece during molding to facilitate the
escape of moisture during baking.
The dough can then be formed into pieces by machining on
a rotary molder with specific die shapes. The dough can also
be formed into pieces by sheeting followed by either a
vertical or rotary cutter or by a rotary molder. Suitable die
and cutter shapes are those which result in a round, square,
triangular, T-bone or chop-shaped biscuit product and the
like. The forming is achieved at conventional temperatures of
ambient to 110F and pressures of less than 75 p.s.i. (gauge),
u~sed with a rotary molder, a vertical cutter or rotary cutter.
The dough pieces can be baked using any suitable or
conventional equipment and conditions. For example, the dough
pieces can be passed into an oven such as a conventional band
oven where the biscuit is baked. The conveyer belts of the
oven can be coated with an edible lubricant such as a natural
or synthetic cooking oil or shortening to facilitate
16
1338179
separation from the conveyer belts of the baked products.
Temperatures in the range of about 300 to about 600F can be
used. The baked biscuits can also be subjected to subsequent
drying at temperatures of about 200 to 400F, either within
the baking oven or separately, to produce the desired
moisture content in the final product.
The formed pieces are baked, followed by drying, to
achieve a shelf stable product without the need of any
moisture barrier protection. Baking and drying temperatures
and times are those conventionally used in the production of a
hard, dry canine biscuit. The pieces are dried to obtain a
biscuit having a water activity of 0.70 or less. Typically,
baking temperatures and times are about 300F to about an
average of 475F for about 25 minutes to about 8 minutes.
Drying conditions are typically about 200 to about 325F for
about 25 minutes to about 12 minutes in a forced air dryer.
On a weight basis, the moisture content of the final biscuit
product is less than or equal to about 15 percent by weight
and preferably about 10 to 12 percent by weight of the final
biscuit at 70 percent relative humidity.
The ingredients, pH and ranges for the invention dough
are the same for the invention dog biscuits.
The invention product is generally as palatable as Milk
Bon ~ dog biscuits, which have been widely accepted and a
commercial success for many years.
The invention product does not include any fluorine-
containing compound or other fluoride ion source, or
~33817!~
quaternary ammonium compounds. Also the invention product
does not include any organic pyrophosphates.
The invention deals primarily with dogs, but has a scope
of teeth-bearing non-human mammals, such as, cats.
The invention composition is used to reduce and control
tartar accumulation on canine teeth. Based upon the weight of
commercial Milk Bon ~ dog biscuits: 12 small invention dog
biscuits per day, 10 medium invention dog biscuits per day, 6
large invention dog biscuits per day or 4 extra large
invention dog biscuits per day will supply about 1/4 to 1/3 of
a dog's caloric requirement.
The invention also involves a process for preparing dog
biscuit dough which is nutritionally balanced and which
contains at least one inorganic pyrophosphate. The process
includes admixing the ingredients of the dog biscuit dough and
the at least one inorganic pyrophosphate. The ingredients and
the at least one inorganic pyrophosphate are selected and
adjusted in amounts which provide a nutritional balance. The
inorganic pyrophosphate also reduces the accumulation of
tartar on the teeth of dogs.
Preferably the dry dough ingredients and the inorganic
pyrophosphate salts are mixed, then water is added and the
mixing continued, and finally the fat (tallow) is added and
thoroughly mixed in.
The dog biscuits can be made from any suitable dough. In
one advantageous embodiment, a bone-shaped canine biscuit is
provided which is baked from a dough comprising wheat flour,
wheat meal, soybean meal, meat and bone meals, animal fat and
18
1~38179
water. The baked dog blscult has an overall molsture content
of 13 weight percent or less.
The composltlons of the dog blscult doughs are mod-
lfied as descrlbed hereln to provlde nutrltlonally-balanced
dog blscults.
The lnventlon also lnvolves dog blscult dough whlch
is nutrltlonally balanced and whlch contalns at least one
lnorganlc pyrophosphate. Generally, the lnventlon dog blscult
dough contalns: about 0.1 to about 7 welght percent of Ca,
about 0.08 to about 6 welght percent of P, about 0.05 to about
3 weight percent of K, about 0.1 to about 3 weight percent of
Na and about 0.15 to about 4.5 welght percent of Cl , prefer-
ably about 0.5 to about 4 welght percent of Ca, about 0.4 to
about 3 welght percent of P, about 0.15 to about 3 welght
percent of K, about 0.2 to about 2.0 welght percent of Na and
about 0.3 to about 3 welght percent of Cl ; and most prefer-
ably about 1.0 to about 2.5 welght percent of Ca, about 0.8 to
about 2.0 welght percent of P, about 0.25 to about 2.0 welght
percent of K, about 0.3 to about 1.0 welght percent of Na and
about 0.45 to about 1.5 welght percent of Cl . The above
welght percentages are based upon the entlre welght of the dog
blscult doughs (or unbaked dog blscults or baked dog bls-
cults), assumlng a water content of 10 welght percent for
these calculatlons. Preferably the ratlo of Ca to P ls
between about 1.0:1 and about 1.6:1, and most preferably the
ratio of Ca to P is between about 1.1:1 and about 1.4:1.
One of the keys to the lnvention ls the selectlon and
ad~ustment ln amounts of the dog blscult dough ingredients and
-- 19 --
~ 73783-60
13381~9
the at least one inorganic pyrophosphate salt to provide a
nutritional balance.
The dog biscuit dough preferably contains about 0.1 to
about 10 weight percent of the at least one inorganic
pyrophosphate compound, and most preferably about 0.5 to about
5 weight percent of said at least one inorganic pyrophosphate
compound. The preferred inorganic pyrophosphate salt(s) is an
alkali metal pyrophosphate. Most preferably the dog biscuit
dough contains a combination of sodium acid pyrophosphate and
tetrapotassium pyrophosphate.
The invention also involves a process for preparing
unbaked dog biscuits from the dog biscuit dough. The
invention also involves unbaked dog biscuits which are
nutritionally balanced and which contain at least one
inorganic pyrophosphate. The dog biscuit pieces preferably
are bone shaped. The unbaked dog biscuits have a moisture
content usually in the range of about 25 to about 40 weight
percent, preferably about 33 to about 35 weight percent.
The invention also involves a process for preparing baked
dog biscuits which are nutritionally balanced and which
contain at least one inorganic pyrophosphate. The process
~ncludes:
(a) shaping a dog biscuit dough, which is nutritionally
balanced and which contains the at least one inorganic
pyrophosphate, into dog biscuit pieces comprising unbaked dog
biscuits; and
(b) baking the unbaked dog biscuits.
133~17~
The baked dog biscuits can be dried, if necessary, to obtain
the desired moisture level. The baked dog biscuits should
have a moisture content of 13 weight percent or less,
advantageously between about 5 and 13 weight percent, and
preferably between about 8 and about 12 weight percent. The
invention product is baked so that it comprises a baked dog
biscuit which is nutritionally balanced and which contains at
least one inorganic pyrophosphate.
The invention further involves baked dog biscuits which
are nutritionally balanced and which contain at least one
inorganic pyrophosphate. The ingredients, ratios, ranges,
etc., for the invention dog biscuit dough applies to the
invention baked dog biscuits except as otherwise noted herein.
The invention product preferably should be slightly acid
to neutral.
The inorganic pyrophosphates are anti-tartar, anti-plaque
or anti-calculus agents. The invention product exhibits anti-
tartar properties over its normal shelf life. The invention
product does not adversely affect canine tooth enamel.
The invention further involves a process for the
prevention or reduction of tartar accumulation on the teeth of
dogs. The process includes the chewing and/or eating of the
invention baked dog biscuits by the dogs. The term "dog
biscuit" herein means a baked dog biscuit unless otherwise
stated herein or otherwise obvious herefrom to one skilled in
the art.
The invention biscuits, when eaten and chewed by dogs,
cleans teeth surfaces, removes tartar (by mechanical action),
1338179
and exercises and massages the gums. The pyrophosphate ln the
lnventlon blscuits prevents or reduces the formation of tartar
on the dog's teeth. The pyrophosphate, in the levels
involved, does not adversely affect the gastrolntestlnal
system or the health of the dogs.
The dog biscuits can be made from any suitable dough,
which is modified as described herein to provide nutrition-
ally-balanced dog blscuits contalning pyrophosphate.
Any suitable dough comprising at least one flour,
meal, fat and water can be employed for the product. For
instance, when the desired product is a canine biscuit, a
conventional dough for dog biscuits can be used, optionally
containing discrete particles of meat and/or meat byproducts
or farinaceous material. Such doughs typically contain fat
solids. Examples of suitable doughs for the production of
hard dog biscuits are disclosed in U.S. Patent No. 4,454,163,
and suitable doughs for the production of soft dog blscuits
~containing humectant to control water activity) are disclosed
in U.S. Patent No. 4,454,164. Particulate proteinaceous
particles, such as, particles of meat, texturized vegetable
proteln and/or meat byproducts, can be incorporated to add
flavor to the blscuits and texturize the surface. Particulate
farinaceous materials, such as, bran particles, can also be
employed to texturlze the interior and/or surface of the
blscuits and to provide other useful properties to the prod-
uct. A dough found to produce blscuits hlghly palatable to
dogs lncludes sultable proportlons of wheat flour, wheat meal,
soybean meal, meat and bone meal, anlmal fat and natural
- 22 -
73783-60
8 1 7 9
flavors ln admlxture wlth water. The meal used in the doughs
suitable for production of biscults useful in the invention
can comprise meat and/or bone andtor vegetable matter includ-
lng farlnaceous materials, materials prepared from legumes
such as beans and peas, tuberous materlals such as potato
meal, and the like. The meals can be finely or coarsely
ground as desired for the texture. Flours made from any
sultable farlnaceous materlal can be used.
The doughs generally have a water actlvlty of about
0.90 and above upon completion of mixing of the dough ingredi-
ents. A suitable dough contains farinaceous material, an
edible oil, an antioxidant, an antimycotlc, salt, anlmal fat,
added vltamlns and mlnerals, such as those disclosed in U.S.
Patent No. 4,229,485, column 5, lines 7 to 57. The composi-
tions of the lnventlon also preferably contain at least one
animal-derived protelnaceous meal such as meat meal, bone meal
and flsh meal. A good biscuit dough for producing the bis-
cults of the invention contains about 50 to 60 percent by
weight of wheat flour, about 5 to 10 percent by weight of
soybean meal, about 3 to 10 percent by weight of meat and bone
meal, about 1 to 5 percent of wheat meal, about 1 to 5 percent
of animal fat preserved with BHA, about 20 to 30 percent by
welght of water, and about 2 to 5 percent by weight of natural
flavors, vitamln and mlneral preblend, and acidulant.
- 23 -
D 73783-60
-
1338179
The dog biscuit doughs are modified as described herein
to provide nutritionally-balanced dog biscuits.
The solvent used in preparing the dog biscuit dough is
preferably water, but other non-toxic, edible solvents, such
as, ethanol or ethanol/water, can be used. The problem of the
necessity of solvent removal from the dough due to toxicity is
to be avoided in most cases. If a mixture of ethanol and
water is used, the amount of ethanol in the mixture is
generally about 5 to about 60 percent, preferably about 5 to
about 25 percent. When one or more of the inorganic
pyrophosphates is not water soluble, it may be ethanol
soluble.
The invention includes the use of at least one inorganic
pyrophosphate. Preferably the inorganic pyrophosphates are
water soluble. A mixture of inorganic pyrophosphates can be
used to help secure a nutritional balance and can be used to
provide a desired pH. The use of water-insoluble or
difficultly soluble inorganic pyrophosphates in a dog biscuit
dough is not a significant problem compared to use of such
materials in a solution, such as, a mouth wash.
The pH of the dough can be adjusted using an inorganic
base (e.g., KOH, NaOH, CaOH, LioH, MgOH, etc.) or an inorganic
acid (e.g., H2SO4, HCl, etc.), but this approach has the
disadvantages of possibly causing a misbalance or
overabundance of one or more chemical entities and possibly
introducing unwanted salts.
24
1338179
Generally 0.1 to 10 weight percent, preferably about 0.5
to about 3.5 weight percent and preferably about 1.4 to about
2.5 weight percent of inorganic pyrophosphate is used.
When a mixture of tetrasodium pyrophosphate (TSPP) and
sodium acid pyrophosphate in aqueous solution at the 5 weight
percent level was incorporated in dog biscuit dough, there was
reduced dough gluten development, the dog biscuits were
bleached (whitish) and crumbly, and the dog biscuits were
softer (a hardness problem) than the control dog biscuits.
Also, such dog biscuits had nutrition problems. At the level
of 3 weight percent of a mixture of tetrasodium pyrophosphate
and sodium acid pyrophosphate, the same problems occurred, but
less severely. The addition of the inorganic pyrophosphates
in dry form to the dry ingredients in the dough preparation
basically eliminated the above problems (except for the
nutrition problem). It was also found that better results
were secured by using the inorganic phosphates in powder form
as opposed to granular form.
The inorganic pyrophosphates are preferably alkali metal
pyrophosphates. The preferred alkali metal pyrophosphates are
tetrasodium pyrophosphate and tetrapotassium pyrophosphate.
An example of useful a tetraalkali metal pyrophosphate is
tetralithium pyrophosphate. Alkaline earth metal
pyrophosphates are also useful, but they are generally
insoluble in water. Preferably the inorganic pyrophosphates
are soluble in water.
Kirk & Othmer, "Encyclopedia Of Chemical Technology", 2nd
Ed., Vol. 15, (1965), pages 232 to 276, discloses a number of
133817g
water-soluble lnorganlc pyrophosphate salts.
Examples of dlalkallne metal pyrophosphates are
dlcalclum pyrophosphate, dlbarlum pyrophosphate and dlmag-
neslum pyrophosphate. Trlalkall metal monoacld pyrophos-
phates, such as, trlsodlum hydrogen pyrophosphate (SAPP), can
be used. Monoalkall metal trlacld pyrophosphates, such as,
sodlum trlhydrogen pyrophosphate, can also be present ln
llmlted amounts. Examples of other lnorganlc pyrophosphates
lnclude manganese pyrophosphate and dlzlnc pyrophosphate.
n+2PnO3n+l, where M ls a unlvalent
metal, ls the formula for unlvalent metal pyrophosphates when
n ls 2. The formula M'nPnO3n+l, where M' ls a dlvalent metal,
ls the formula for dlvalent metal pyrophosphates when n ls 2.
Such unlvalent metal pyrophosphates and dlvalent metal pyro-
phosphates can be used ln the lnventlon. Polyphosphates
have the formula Mn+2PnO3n+l or M nPn3n+1
5,..., and the oxlde ratlo R between the catlonlc oxldes (M2O
or M'O) and anlonlc oxldes (P2O5) ls between 1 and 2. The
oxlde ratlo for pyrophosphate ls 2.
Tetrasodlum pyrophosphate, one part, ls soluble ln 13
parts of cold water and ln 2.5 parts of bolllng water. It ls
lnsoluble ln ethanol. Dlcalclum pyrophosphate ls practlcally
lnsoluble ln water. The lnventlon use of the term "solutlon"
lncludes slurrles, suspenslons and the llke. Tetrapotasslum
73783-60
133817~
pyrophosphate is freely soluble in water and is insoluble in
ethanol.
Most preferably a mixture of sodium acid pyrophosphate
and tetrapotassium pyrophosphate is used (in a ratio to
achieve the desired nutritional delivery and the desired pH).
In such most preferred mixture, tetrasodium pyrophosphate is
not used as it would provide too much sodium in the
nutritionally-balanced composition.
The maximum allowable GRAS level in the U.S. in a
composition for sodium acid pyrophosphate (SAPP) is 2.1 weight
percent and tetrapotassium pyrophosphate (TKPP) is 1.4 weight
percent in baked goods. If GRAS levels change (rise) or if
higher levels are allowed by the regulatory agencies, higher
levels can be used in the invention. TKPP delivers
approximately 52.65 percent of P2O7; SAPP delivers about 78.36
percent of P207; and TSPP delivers about 65.4 percent of P207.
With the total amount of Na and Cl in the dog biscuit
dough (or baked dog biscuit) being taken as 100 weight
percent, preferably the Na content ranges between about 30 and
about 50 weight percent and the Cl- content ranges between
about 50 and about 70 weight percent, and most preferably the
~a content is about 40 to about 44 weight percent and the Cl--
content is about 60 to about 56 weight percent.
The pyrophosphate(s) is used in sufficient amount to
deliver generally from about 0.1 to about 5, preferably from
about 0.5 to about 3.5 weight percent, most preferably 1.4 to
2.5 weight percent (based on the total composition), of P207.
27
13381~ ~
The use of 3.5 welght percent of lnorganic pyrophosphate
salt(s) means the delivery of about 2.5 welght percent of
P207 ~
A study of the appllcatlon of aqueous solutlons of a
mlxture of tetrasodlum pyrophosphate and sodium acld pyrophos-
phate to the teeth of dogs by spraylng for one month resulted
ln dose response data. The aqueous solutlons contalnlng 5 and
3 welght percent of a mixture of tetrasodlum pyrophosphate and
sodlum acld pyrophosphate resulted ln slgnlflcant reductlons
ln tartar accumulatlon. The aqueous solutlons contalnlng 1.5
and 0.5 weight percent of a mlxture of sodlum acld pyrophos-
phate and tetrasodlum pyrophosphate resulted ln dlrectlonal
trends of reductlons ln tartar accumulatlon. See also U.S.
Patent No. 3,323,551.
The ratlo of sodlum acld pyrophosphate (SAPP) to
tetrapotasslum pyrophosphate (TKPP) ls generally between 4 to
1 and 3 to 7, preferably between 7 to 3 and 1 to 1, most
preferably about 3 to about 2. SAPP has a pH of 4.2 and TKPP
(and TSPP) has a pH of 10.2, so the combinatlon of SAPP and
TKPP (or TSPP) provldes a resultant pH whlch ls a balance of
the pHs of the two components.
The pH of the dough contalnlng at least one lnorganlc
pyrophosphate salt (and baked dog blscult) ls generally ln the
range of about 4 to about 10.5, typlcally from about 4.5 to
about 7.5, preferably from about 5 to about 7, most preferably
between about 5.6 and about 6.1. Mllk ~30ne~ dog blscult has a
pH of 6.1 to 6.4. Tartar reductlon ls lndlcated to be best at
neutral pH and palatablllty ls lndicated to be best at a
- 28 -
73783-60
13381~ 9
slightly acidic pH, so the best mode contemplates a balance of
such two factors ln any commerclal product.
The dough ingredlent ls generally mlxed at a tempera-
ture of about 45 to about 140F, preferably about 60 to
about 125F.
The nutritlonally-balanced dog blscult dough gen-
erally contalns about 0.1 to about 7 welght percent of Ca,
about 0.08 to about 6 welght percent of P, about 0.05 to about
3 welght percent of K, about 0.1 to about 3 welght percent of
Na and about 0.15 to about 4.5 welght percent of Cl . The
nutritionally-balanced dog blscuit dough preferably contalns
about 0.5 to about 4 welght percent of Ca, about 0.4 to about
3 welght percent of P, about 0.15 to about 3 welght percent of
K, about 0.2 to about 2 welght percent of Na and about 0.3 to
about 3 welght percent of Cl , and most preferably contalns
about 1.0 to about 2.5 welght percent-of Ca, about 0.8 to
about 2.0 welght percent of P, about 0.25 to about 2.0 welght
percent of K, about 0.3 to about 1.0 weight percent of Na and
about 0.45 to about 1.5 welght percent of Cl . The above
welght percentages are based upon the entire weight of the dog
biscuit doughs (or unbaked dog blscults or baked dog bls-
cults), assumlng a water content of 10 percent for these
calculations. Mlnor nutrltlonal elements can also be ad~usted
as deslred.
The lnventlon is ln llne wlth the nutrltlonal
requlrements of dogs for malntenance as regards calcium,
phosphorus, potasslum, sodlum and chlorlne. Examples lO and
11 are also nutrltlonally complete wlth regard to
- 29 -
73783-60
1~38179
micronutrients. Puppies need high Ca and P for growth. Milk
Bone~ dog biscuits are nutritionally balanced.
The ratio of Ca to P in the nutritionally-balanced dog
biscuit dough is generally, preferably between about 1.0:1 and
about 1.6:1, and most preferably between about 1.2:1 and about
1.4:1.
The critical factor in the prevention or reduction of
tartar accumulation is the pyrophosphate moiety. The
nutritional balance partially depends upon the amounts and
ratios of elements and ions, such as Ca, P, K, Na and Cl-.
The reason that it is best to use tetrapotassium
pyrophosphate, instead of tetrasodium pyrophosphate, with
sodium acid pyrophosphate is that such action holds down the
sodium level in the dough.
In order to provide sufficient calcium to achieve
nutritional balance, calcium carbonate and calcium chloride
are included in the preferred invention formula. It is
advantageous to use calcium chloride (to raise the chlorine
level) and a high level of calcium carbonate instead of the
dicalcium phosphate and the low level of calcium carbonate
used in Milk Bone~ dog biscuits. Also, since the invention
uses pyrophosphates, the P level could be too high if
dicalcium phosphate is also used. The calcium chloride
supplies Cl- to help achieve nutritional balance. The calcium
chloride can be replaced by dicalcium pyrophosphate (with a
corresponding adjustment of the other pyrophosphate salts and
possible addition of another chlorine source). The bone meal
1338179
level in Milk Bon ~ dog biscuits has been lowered in the
preferred invention formula.
The invention biscuits do not include the salt present in
Milk Bon ~ dog biscuits.
The dough can also contain suitable surfactants or
emulsifying agents, best used in minor amounts.
The dog biscuit dough can be mixed using any suitable or
conventional equipment. For example, the mixing can be at 20
to 100 rpm. For example, a dry blending step (dries and the
inorganic pyrophosphates) can be done typically at room
temperature for a period of time of about 3 minutes to about
20 minutes. The dry-blended mixture can then be mixed with
the hot water to form a first stage dough. The water which
can be admixed with the dry-blended mixture is typically at a
temperature of about 65 to about 150F. The hot water can be
added, with mixing, over a period of time of about 3 minutes
to about 6 minutes to form the first stage dough. Then, the
fat portion of the biscuit dough can be admixed with the first
stage dough to form the final stage dough. The fat portion
can be added at a temperature at which it is at least fluid,
typically at about 100 to about 150F. The fat portion can be
~ixed for a period of time which is sufficient to form a dough
whose homogeneity is visually apparent. A typically final
mixing time is about 3 to about 5 minutes.
Initially, there were machinability and dough structure
property problems with the invention dough, but the addition
of water solved such problems. But the use of the higher
water levels caused the dough to be so sticky as to cause
1~3817~
problems in a sigma or rotary mixer (but it is normally not a
slgnlflcant problem ln a continuous mlxer). The addltlon of
more tallow to the dog blscult dough assisted ln more effec-
tlve mlxlng and helped to keep the dough from belng so stlcky
that lt cllngs to the rotary molder. Preferably the tallow
level ls about 2.6 to about 3.1 welght percent ~most preferab-
ly about 2.85 welght percent), as opposed to a tallow level of
about 2.46 welght percent ln Mllk Bone~ dog blscults. Also,
the tallow provldes a taste whlch dogs llke.
Formatlon of the dough ls achleved at about atmos-
pherlc pressure wlth mlxing of the components being conveni-
ently achleved in an uprlght slgma blade mixer or other
bakery-type mixers. The various ingredlents can be added over
a period of tlme or ln a one-shot manner accordlng to the
above order of addltion. However, melted fat and water can be
added slmultaneously and mlxed for 6 to 10 mlnutes.
The dog blscults are formed ln any conventlonal or
sultable manner, such as, by extruslon, stamplng, cuttlng or
moldlng. Any sultable dog blscult shapes can be used, such
as, a bone-shaped canlne blscult. For many products, such as,
the bone-shaped canlne blscults of the lnventlon, a rotary
molding system ls preferred because lt permlts the rapld
formlng of dough pleces wlth good control over thelr shape,
form and surface characterlstlcs. Docker holes are preferably
formed ln the dough plece durlng moldlng to facllltate the
escape of molsture durlng baklng.
The dough can then be formed lnto pleces by machlnlng
on a rotary molder wlth speclflc dle shapes. The dough can
- 32 -
D 73783-60
1338179
also be formed lnto pieces by sheetlng followed by either a
vertlcal or rotary cutter or by a rotary molder. Suitable die
and cutter shapes are those which result in a round, square,
trlangular, T-bone or chop-shaped biscult product and the
llke. The formlng ls achleved at conventlonal temperatures of
amblent to 110F and pressures of less than 75 p.s.l. (gauge),
used wlth a rotary molder, a vertical cutter or rotary cutter.
The dough pleces can be baked uslng any sultable or
conventional equlpment and conditlons. For example, the dough
pleces can be passed lnto an oven such as a conventlonal band
oven where the blscuit ls baked. The conveyer belts of the
oven can be coated wlth an edlble lubricant such as a natural
or synthetlc cooking oil or shortenlng to facilitate separ-
ation from the conveyer belts of the baked products. Tempera-
tures ln the range of about 300 to about 600F can be used.
The baked biscults can also be sub~ected to subsequent drying
at temperatures of about 200 to 400F, either wlthln the
baklng oven or separately, to produce the deslred molsture
content ln the flnal product.
The formed pleces are baked, followed by drylng, to
achieve a shelf stable product wlthout the need of any mols-
ture barrler protectlon. Baklng and drylng temperatures and
tlmes are those conventlonally used in the productlon of a
hard, dry canlne blscult. The pleces are drled to obtaln a
blscult havlng a water actlvlty of 0.70 or less. Typlcally,
baklng temperatures and tlmes are about 300F to about an
average of 475F for about 25 mlnutes to about 8 mlnutes.
Drylng condltions are typlcally about 200 to about 325F for
- 33 -
73783-60
13~8179
about 25 minutes to about 12 minutes in a forced air dryer.
On a weight basis, the moisture content of the final biscuit
product is less than or equal to 13 percent by weight, usually
at least 5 weight percent, and most preferably about 8 to
about 12 percent by weight, of the final biscuit at 70 percent
relative humidity.
The ingredients, pH and ranges for the invention dough
are the same for the invention dog biscuits.
The invention product is similar as palatable as Milk
Bon ~ dog biscuits, which have been widely accepted and a
commercial success for many years.
The invention product does not include any fluorine-
containing compound or other fluoride ion source, or
quaternary ammonium compounds. Also the invention product
does not include any organic pyrophosphates.
The invention deals primarily with dogs, but has a scope
of teeth-bearing non-human mammals, such as, cats.
The invention composition is used to reduce and control
tartar accumulation on canine teeth. Based upon the weight of
commercial Milk Bon ~ dog biscuits: 12 small invention dog
biscuits per day, 10 medium invention dog biscuits per day, 6
large invention dog biscuits per day or 4 extra large
invention dog biscuits per day will supply about 1/4 to 1/3 of
a dog's caloric requirement.
The following table sets out the content of nutritionally
important elements and ions in various dog biscuits:
34
1338179
Table 1
1.6% 2.34%
Pyrophosphate Pyrophosphate
Milk Bon ~ Example lla Example 10
Elements Dog Biscuits Dog Biscuits Dog Biscuits
Or Ions Wt. Percent Wt. Percent Wt. Percent
Ca 1.21 1.581 1.843
P 0.978 1.333 1.585
K 0.846 1.105 1.252
Na 0.413 0.488 0.516
Cl-- 0.524 0.651 0.662
OTES: 1. Milk Bone~ is a registered trademark of Nabisco Brands,
Inc. for canine biscuits.
2. The ratio of Ca to P is 1.1-1.2 to 1 in Milk Bon ~ canine
biscuits.
3. The weight percentages are based on the final canine
biscuits having a moisture content of 10 percent.
4. The Examples 10, lla and llb formulas are the most
preferred compositions.
It is most preferred to have a chlorine content of about
40 to about 44 weight percent and a Na content of about 60 to
about 56 weight percent, based on the total weight of Na and Cl
in the dog biscuit. The most preferred calcium/phosphorus ratio
of 1.1-1.4:1 is best for growth and maintenance.
The invention also includes a process for preparing dog
biscuit dough having a coating containing at ~east one inorganic
pyrophosphate compound, which includes preparing a dog biscuit
dough, forming the dog biscuit dough into pieces, subjecting the
dog biscuit dough pieces to a liquefied coating material having
at least one inorganic pyrophosphate, thereby forming a coating
of such liquefied coating material on the dog biscuit dough
pieces, and baking (and optionally drying) the dog biscuit dough
pieces having a coating containing at least one inorganic
13381~9
pyrophosphate. The lnorganlc pyrophosphate reduces the accu-
mulatlon of tartar on the teeth of dogs.
Preferably the dry dough ingredlents are mixed, then
water ls added and the mlxlng contlnued, and finally the fat
(tallow) ls added and thoroughly mlxed ln. The dog blscults
can be made from any sultable dough. In one advantageous
embodiment, a bone-shaped canlne blscult ls provlded whlch ls
baked from a dough comprlslng wheat flour, wheat meal, soybean
meal, meat and bone meals, animal fat and water. The baked,
coated biscult has an overall molsture content of 13 welght
percent or less.
The coatlng on the dog blscult dough preferably
contalns about 0.1 to about 10 welght percent of the at least
one lnorganlc pyrophosphate compound, and most preferably
about 0.5 to about 5 welght percent of sald at least one
inorganic pyrophosphate compound. The preferred lnorganic
pyrophosphate salt(s) ls an alkall metal pyrophosphate. Whlle
the preferred alkall metal pyrophosphate ls tetrasodlum
pyrophosphate, most preferably the dog blscult dough contalns
a comblnatlon of trlsodlum monoacld pyrophosphate and
tetrapotasslum pyrophosphate (or tetrasodlum pyrophosphate).
The lnvention also involves unbaked dog blscuits
whlch have a coatlng whlch contalns at least one lnorganlc
pyrophosphate. The dog blscult pleces preferably are bone
shaped. The unbaked dog blscuits preferably have a moisture
content usually ln the range of about 25 to about 40 welght
percent, preferably about 33 to about 35 welght percent.
- 36 -
73783-~0
1 7 9
The invention also involves a process for preparing baked
dog biscuits which have a baked coating containing at least one
inorganic pyrophosphate. The process includes:
(a) placing a coating, balanced and which contains the at
least one inorganic pyrophosphate, onto unbaked dog biscuit
dough pieces comprising unbaked dog biscuits; and
(b) baking the coated, unbaked dog biscuits.
The baked dog biscuits can be dried, if necessary, to obtain the
desired moisture level. The baked dog biscuits should have a
moisture content of 13 weight percent or less, advantageously
between 5 and 13 weight percent, and preferably between about 8
and about 12 weight percent.
The invention product is baked so that it comprises a baked
dog biscuit which has a coating containing at least one
inorganic pyrophosphate.
The invention further involves baked, coated dog biscuits,
such coating containing at least one inorganic pyrophosphate.
The ingredients, ratios, ranges, etc., for the invention dog
biscuit dough and coating applies to the invention baked, coated
dog biscuits, except as otherwise noted herein.
The invention product (including coating) should be
s~lightly acid to neutral.
The inorganic pyrophosphates are anti-tartar, anti-plaque
or anti-calculus agents. The invention product exhibits
anti-tartar properties over its normal shelf life. The
invention product does not adversely affect canine tooth enamel.
The invention further involves a process for the prevention
or reduction of tartar accumulation on the teeth of dogs. The
133817~
process includes the chewing and/or eatlng of the lnventlon
baked, coated dog blscults by the dogs.
The lnventlon blscults, when eaten and chewed by
dogs, cleans teeth surfaces, removes tartar (by mechanlcal
actlon), and exerclses and massages the gums. The pyrophos-
phate ln the coatlng of the lnventlon blscults prevents or
reduces the formatlon of tartar on the dog's teeth. The
pyrophosphate, ln the levels lnvolved, does not adversely
affect the gastrolntestlnal system or the health of the dogs.
The dog blscults can be made from any sultable dough,
whlch ls modlfied as descrlbed hereln to provlde nutrltlon-
ally-balanced dog blscults contalnlng pyrophosphate.
Any sultable dough comprlslng at least one flour,
meal, fat and water can be employed for the coated product.
For lnstance, when the deslred product ls a canlne blscuit, a
conventlonal dough for dog blscults can be used, optlonally
contalnlng dlscrete partlcles of meat and/or meat byproducts
or farlnaceous materlal. Such doughs typlcally contaln fat
sollds. Examples of sultable doughs for the productlon of
Z0 hard dog blscuits are dlsclosed ln U.S. Patent No. 4,454,163,
and sultable doughs for the productlon of soft dog blscults
(contalnlng humectant to control water actlvlty) are dlsclosed
ln U.S. Patent No. 4,454,164. Partlculate protelnaceous
partlcles, such as, partlcles of meat, texturlzed vegetable
proteln and/or meat byproducts, can be lncorporated to add
flavor to the blscults and texturlze the surface. Partlculate
farlnaceous materlals, such as, bran partlcles, can also be
employed to texturlze the surface of the blscults and to
provlde other useful propertles to the product. A dough found
- 38 -
73783-60
133817~
to produce blscuits highly palatable to dogs lncludes sultable
proportlons of wheat flour, wheat meal, soybean meal, meat and
bone meal, animal fat and natural flavors in admixture with
water. The meal used ln the doughs sultable for productlon of
biscults useful in the lnvention can comprise meat and/or bone
and/or vegetable matter lncluding farlnaceous materlals,
materlals prepared from legumes such as beans and peas, tuber-
ous materlals such as potato meal, and the llke. The meals
can be finely or coarsely ground as desired for the texture.
Flours made from any suitable farlnaceous materlal can be
used.
The doughs generally have a water actlvlty of about
0.90 and above upon completlon of mixlng of the dough ingredi-
ents. A suitable dough contains farinaceous material, an
edible oil, an antioxidant, an antimycotlc, salt, animal fat,
added vltamlns and mlnerals, such as those dlsclosed in U.S.
Patent No. 4,229,485, column 5, llnes 7 to 57. The composl-
tions of the lnventlon also preferably contain at least one
animal-derlved proteinaceous meal such as meat meal, bone meal
and fish meal. A good biscuit dough for producing the bis-
cuits of the invention contains about 50 to 60 percent by
weight of wheat flour, about 5 to 10 percent by weight of
soybean meal, about 3 to 10 percent by weight of meat and bone
meal, about 1 to 5 percent of wheat meal, about 1 to 5 percent
of animal fat preserved with BHA, about 20 to 30 percent by
weight of water, and about 2 percent by weight of natural
flavors, vitamin and mlneral preblend, and acldulant.
The dough can also contaln sultable surfactants or
emulslfying agents, e.g., whlch are best used ln mlnor
- 39 -
73783-60
amounts. 133817 9
The dog biscult dough can be mlxed uslng any sultable
or conventlonal equlpment. For example, the mlxlng can be at
20 to 100 rpm. For example, a dry blending step can be done
typically at room temperature for a perlod of tlme of about 3
mlnutes to about 10 mlnutes. The dry-blended mlxture can then
be mlxed wlth the hot water to form a flrst stage dough. The
water whlch can be admixed wlth the dry-blended mlxture is
typlcally at a temperature of about 65 to about 150F. The
hot water can be added, with mixing, over a perlod of tlme of
about 3 mlnutes to about 5 mlnutes to form the flrst stage
dough. Then, the fat portlon of the blscult dough can be
admlxed wlth the flrst stage dough to form the flnal stage
dough. The fat portlon can be added at a temperature at which
it is at least fluid, typically at about 100 to about 150F.
The fat portion can be mixed for a period of time whlch ls
sufficient to form a dough whose homogeneity ls vlsually
apparent. A typically flnal mixlng tlme ls about 3 to about 5
minutes.
Formatlon of the dough ls usually achleved at about
atmospherlc pressure wlth mlxlng of the components belng
convenlently achleved ln an uprlght slgma blade mlxer or other
bakery-type mlxers. The varlous lngredlents can be added over
a perlod of tlme or ln a one-shot manner accordlng to the
above order of addltlon. However, melted fat and water can be
added slmultaneously and mlxed from 6 to lO mlnutes.
The dog blscults are formed ln any conventlonal or
sultable manner, such as, by extruslon, stamplng, cuttlng or
moldlng.
- 40 -
73783-60
133~179
Any suitable dog biscuit shapes can be used, such as, a
bone-shaped canine biscuit. For many products, such as, the
bone-shaped canine biscuits of the invention, a rotary molding
system is preferred because it permits the rapid forming of
dough pieces with good control over their shape, form and
surface characteristics. Docker holes are preferably formed in
the dough piece during molding to facilitate the escape of
moisture during baking.
The dough can be then formed into pieces by machining on a
rotary molder with specific die shapes. The dough can also be
formed into pieces by sheeting followed by either a vertical or
rotary cutter or by a rotary molder. Suitable die and cutter
shapes are those which result in a round, square, triangular,
T-bone or chop-shaped biscuit product and the like. The forming
is achieved at conventional temperatures of ambient to 110F and
pressures of less than 75 p.s.i. (gauge), used with a rotary
molder, a vertical cutter or rotary cutter.
The solvent used in the coating is preferably water, but
other non-toxic, edible solvents, such as, ethanol or
ethanol/water, can be used. The problem of the necessity of
solvent removal from the coated dough due to toxicity is to be
~voided in most cases. If a mixture of ethanol and water is
used, the amount of ethanol in the mixture is generally about 5
to about 60 percent, preferably about 5 to about 25 percent.
when one or more of the inorganic pyrophosphates is not water
soluble, it may be ethanol soluble.
The invention includes the use of at least one inorganic
pyrophosphate. Preferably the inorganic pyrophosphates are water
41
1338179
soluble. A mixture of inorganic pyrophosphates can be used to
provide a desired pH. The use of a water insoluble inorganic
pyrophosphate, by itself or in a mixture, (along with the other
water insoluble ingredients) results in a slurry. The use of
very fine particles of a water insoluble inorganic pyrophosphate
provides better suspension in the coating formulation.
The inorganic pyrophosphates are preferably alkali metal
pyrophosphates. The preferred alkali metal pyrophosphate is
tetrasodium pyrophosphate and tetrapotassium pyrophosphate. An
example of useful tetraalkali metal pyrophosphates is
tetralithium pyrophosphates. Alkaline earth metal pyrophosphates
are also useful, but they are generally insoluble in water.
Preferably the inorganic pyrophosphates are soluble in
water.
The formula Mn+2PnO3n+, where M is a univalent metal, is the
formula for univalent metal pyrophosphates when n is 2. The
formula M'nPnO3n+~ or where M' is a divalent metal, is the formula
for divalent metal pyrophosphates when n is 2. Such univalent
metal pyrophosphates and divalent metal pyrophosphates can be
used in the invention. Polyphosphates have the formula Mn+2PnO3n+~
or M'nPnO3n+~. where n is 2, 3, 4, 5, ..., and the oxide ratio R
~etween the cationic oxides (M20 or M'O) and anionic oxides (P205)
is between 1 and 2. The oxide ratio for pyrophosphate is 2.
Generally 0.1 to 10 weight percent, advantageously about 0.5
to about 5 weight percent and preferably about 1.5 to about 3
weight percent of inorganic pyrophosphate is used.
Kirk & Othmer, "Encyclopedia Of Chemical Technology", 2nd
Ed., Vol. 15, (1965), pages 232 to 276, discloses a number of
42
1338179
water-soluble lnorganlc pyrophosphate salts.
Examples of dlalkallne metal pyrophosphates are
dlcalclum pyrophosphate, dlbarlum pyrophosphate and dlmag-
neslum pyrophosphate. Trlalkall metal monoacld pyrophos-
phates, such as, trlsodlum hydrogen pyrophosphate (SAPP), can
be used. Monoalkall metal trlacld pyrophosphates, such as,
sodium trlhydrogen pyrophosphate, can also be present ln
llmlted amounts. Examples of other lnorganlc pyrophosphates
include dlmanganese pyrophosphate and dlzlnc pyrophosphate.
Tetrasodlum pyrophosphate, one part, ls soluble ln 13
parts of cold water and ln 2.5 parts of bolllng water. It ls
lnsoluble ln ethanol. Dlcalclum pyrophosphate ls practlcally
lnsoluble ln water. The lnventlon use of the term "solutlon"
lncludes slurrles, suspenslons and the llke. Tetrapotasslum
pyrophosphate ls freely soluble ln water and ls lnsoluble ln
ethanol.
The lnventlon product does not lnclude any
fluorlne-contalnlng compound or other fluorlde lon source, or
guaternary ammonlum compounds. The lnventlon does not lnclude
organlc acid pyrophosphates.
More preferably a mixture of trisodium monoacld
pyrophosphate and tetrapotasslum pyrophosphate is used ~in a
ratio to achieve the desired pH).
The maximum allowable GRAS level in the U.S. In a
composition for sodlum acld pyrophosphate (SAPP) ls 2.1 weight
percent and for tetrapotasslum pyrophosphate (TKPP) or
- 43 -
73783-60
. 1338179
.
tetrasodium pyrophosphate (TSPP) 1.4 weight percent in baked
goods. If GRAS levels change (rise) or if higher levels are
allowed by the regulatory agencies, higher levels can be used in
the invention. TSPP delivers about 65.4 percent by P207, TKPP
delivers about 52.65 percent of P207 and SAPP delivers about
78.36 percent of P207.
The preferred invention coating contains trisodium monoacid
pyropho~;phate and tetrapotassium pyrophosphate in a weight ratio
of about: 60 to about 40.
Th~ pyrophosphate(s) is used in sufficient amount to
deliver generally from about 0.1 to about 5, preferably from
about 3.5, most preferably 1.4 to 2.5 weight percent (based on
the total composition), of P207.
A study of the àpplication of aqueous solutions of a
mixture of tetrasodium pyrophosphate and sodium acid
pyrophosphate to the teeth of dogs by spraying for one mouth
resulted in dose response data. The aqueous solutions
containing 5 and 3 weight percent of a mixture of tetrasodium
pyrophosphate and sodium acid pyrophosphate resulted in
significant reductions in tartar accumulation. The aqueous
solutions containing 1.5 and 0.5 weight percent of such mixture
resulted in directional trends of reductions in tartar
a~cumula~tion. See also U.S. Patent No. 3,323,551.
The ratio of sodium acid pyrophosphate (SAPP) to
tetrapotassium pyrophosphate (TKPP) is between 4 to 1 and 3 to
7, preferably between 7 to 3 and 1 to 1, most preferably about 3
to about 2. SAPP has a pH of 4.2 and TKPP (and TSPP) has a pH
of 10.2, so the combination of SAPP and TKPP (or TSPP) provides
44
133817 9
a resultant pH which is a balance of the pHs of the two
components. The pH of the coating solution of at least one
inorganic pyrophosphate salt (and baked, coated dog biscuit) is
generally in the range of about 4 to about 10.5, typically from
about 4.5 to about 7.5, preferably from about 5 to 7, most
preferably about 5.6 to 6.1. Milk Bone has a pH of 6.1 to 6.4.
Tartar reduction is indicated to be best at neutral pH and
palatability is indicated to be best at a slightly acidic pH, so
the best mode contemplates a balance of such two factors in any
commercial product. The coating solution application is usually
conducted at a temperature of about 45 to about 140F,
preferably about 60 to about 125F.
The coating solution contains a suitable surfactant. The
preferred surfactant is lecithin or a modified lecithin, most
preferably a modified lecithin which is in a dry form.
Preferably about 0.5 to about 1.75 weight percent of the
lecithin or modified lecithin is used. The surfactant or
wetting agent helps the coating material to apply over the
entire surface of the dog biscuit dough pieces. The liquefied
coating formulation best contains at least one suspension agent.
The preferred suspension agent is a polysaccharide gum.
`Preferably about 0.05 to 1.25 weight percent of xanthan gum is
used. Xanthan gum is one of the few gums which acts as an
acceptable suspension agent in the invention. Any suitable gums
and mucilages can be used. Xanthan gum is preferred because it
is stable over a broad range of temperature and holds the same
viscosity in the liquefied coating formulation over the broad
temperature range. The xanthan gum has a bodying effect so that
1338l7~
little or no separation occurs. Malto-dextrin produced by
hydrolyzing corn starch is preferred. It serves as a carrier
(bodying), binding agent and suspension agent and helps the
appearance of the coating. It is a preferred ingredient, but
any suitable dextrin can be used in its place. Other
malto-dextrins can also be used for the same functions.
An adhesive or binding agent, such as, malto-dextrins, is
needed in the coating slurry to help the coating material bind
(adhere) to the dog biscuit when the dog biscuit is dipped in
the coating slurry. Preferably about 5 to about 15 weight
percent of the-dextrin or malto-dextrin is included in the
coating material.
A carrier, such as, starch or a modified food starch, is
included in the coating formulation. Preferably about 0.1 to
about 5 weight percent of the food starch or modified food
starch is included in the coating material. The food starch or
modified food starch also serves to control the viscosity.
Animal fat preferably is included for flavor purposes.
Other suitable flavorants can be included, particularly salt.
The flavorants can be any dairy product flavorant, such as, milk
or cheese, meat flavorants, such as, liver or beef, poultry and
fish. Flavorants help provide palatability for the invention
coating.
Preferably a hydrogenated vegetable oil is included in the
coating formulation for sheen and to modify the melting point of
the formula fats in the finished product. It also helps to
prevent flaking of the coating; also the coating does not have a
tacky feeling.
46
1338179
Any suitable colorant can be included in the coating
formulation. The preferred colorant is caramel color, which
also provides some flavor to the product.
The coating also incorporates sufficient water to achieve
the liquefied coating composition. Amounts of the other
ingredients are those which are effective to achieve their
functions in the coating formulation. The preferred coating
formulation, besides the inorganic pyrophosphates, contains
animal fat, a surfactant, such as, a modified lecithin,
polysaccharide gum, a modified food starch, flavorant, colorant,
hydrogenated vegetable oil, a carrier, such as a malto-dextrin,
and water.
The coating slurry can be applied to the dog biscuit dough
pieces by any suitable means, such as, spraying, dipping,
soaking in a container, etc. The coating slurry is applied
generally at a temperature of 45 to 200F, preferably at about
60 to about 190F, and most preferably at about 180. The
coating slurry has a low microbial profile at such higher
temperatures.
The coated dough pieces can be baked using any suitable or
conventional equipment and conditions. For example, the coated
~ough pieces can be passed into an oven such as a conventional
band oven where the biscuit is baked. The conveyor belts of the
oven can be coated with an edible lubricant such as a natural or
synthetic cooking oil or shortening to facilitate separation
from the conveyor belts of the baked coated products.
Temperatures in the range of about 300 to about 600F can be
used. The baked coated biscuits can also be subjected to
47
13~8179
subsequent drying at temperatures of about 200 to 400F, either
within the baking oven or separately, to produce the desired
moisture content in the final product.
The coated, formed pieces are baked, followed by drying, to
achieve a shelf stable product without the need of any moisture
barrier protection. Baking and drying temperatures and times
are those conventionally used in the production of a hard, dry
canine biscuit. The pieces are dried to obtain a biscuit having
a water activity of 0.70 or less. Typically baking temperatures
and times are about 300F to about an average of 475F for about
25 minutes to about 8 minutes. Drying conditions are typically
about 200 to about 325F for about 25 minutes to about 12
minutes in a forced air dryer. On a weight basis, the moisture
content of the final coated biscuit product is less than or
equal to 13 percent by weight, usually at least 5 weight
percent, and most preferably about 8 to about 12 percent by
weight, of the final biscuit at 70 percent relative humidity.
The ingredients, pH and ranges for the invention coated
dough are the same for the invention coated dog biscuits. The
invention product is similar in palatability to Mil ~ dog
biscuits, which have been widely accepted and a commercial
success for many years.
The invention product does not include any fluorine-
containing compound or other fluoride ion source, or quaternary
ammonium compounds. Also the invention product does not include
any organic pyrophosphates.
The invention deals primarily with dogs, but has a scope of
teeth-bearing non-human mammals, such as, cats.
48
1~38179
The invention composition is used to reduce and control
tartar accumulation on canine teeth.
49
1338179
The following coating-baking procedure is particularly
advantageous:
(a) dry blending the dry powders.
(b) adding 1/4 of the water and slurring the composition.
(c) adding remaining 3/4 of the water and mixing to form
the coating formulation.
(d) heating the coating formulation to 185 to 200F with
intermittent stirring (add animal fat at about 125F
during the heating).
(e) maintaining the coating formulation at 160 to 190F.
(f) apply the coating material to the unbaked dough
pieces.
(g) baking the coated, unbaked dough pieces at 325F for
25 minutes.
(h) drying the baked, coated dough pieces for 25 minutes
at 225F in a forced-air dryer.
The invention also includes a process for preparing raw
hide containing at least one inorganic pyrophosphate compound,-
comprising:
(a) subjecting raw hide to a solution containing at least
one inorganic pyrophosphate compound; and
(b) drying the raw hide containing said at least one
inorganic pyrophosphate compound.
The invention further includes raw hide containing at least
one inorganic pyrophosphate salt. The invention also includes a
process for the prevention of tartar accumulation on the teeth
of dogs comprising chewing and/or eating the treated raw hide.
51
1338179
The preferred coating formulation is:
Table 2
Ingredients Percentages
Specific Ranqes
Sodium acid pyrophosphate (SAPP),
anhyd:rous powder, (non-leavening
type) 1.73 0.25 to 5
Tetrapotassium pyrophosphate
(TKPP), anhydrous powder 1.15 0.25 to 5
Salt 0.50 0.05 to 2.5
Malto-Dextrin 9.17 2 to 30
Modified Food Starch 2.00 0.1 to 10
Colorant 0.50 0.01 to 3
Flavorant 2.00 0.01 to 5
Xanthan 0.20 0.05 to 1.5
Lecithin or Modified Lecithin1.25 0.5 to 1.75
Vegetable Fat 0.50 0.1 to 3
Animal Fat 1.00 0.1 to 5
Subtotal20.00
Water (assumed completely
evaporated after drying) 80.00 50 to 97
Total 100.00
1~38179
In the preparation of raw hide, the skin that is made into
raw hide should not be salted: instead, it is softened with
water and immersed in a dehairing solution made, for example, by
combining 2-1/2 pounds of slaked caustic lime with ten gallons
of water. The skin is left in the solution until the hair slips
very easily, and then it is removed and rinsed in clean water.
After letting the skin drain, it is put on the fleshing beam and
the hair is scraped off as well as the epidermis layer of skin
under the hair. When the hair is gone, the hide is turned over
and fleshed very well, removing every bit of flesh and fat.
Then the hide is soaked for a while in clean water to wash away
all dirt and bits of material removed by the fleshing and
dehairing operations. The hide is stretched on a frame and
allowed to air dry.
More generally, hair removal can be accomplished with a
saturated solution of calcium hydroxide (lime) alone or in
combination with a sharpening agent, e.g., sodium sulfide or
sodium sulfhydrate. Lime by itself does not dissolve the hair
but only loosens it in the base of the hair follicle for easy
removal by an unhairing machine. This labor-intensive apparatus
scrapes the loosened hair from the surface of the skin and is
~ermed a hair-save process. Lime, by itself, requires from 5 to
7 days to loosen the hair. Because of the importance of time, a
hair-burn process is more commonly used. Although sulfide at a
pH greater than 11.5 can dissolve the hair in as little as 30 to
40 minutes, the usual sulfide unhairing process takes from 4 to
6 hours.
1~3817~
The dehairing scheme using ultrasonic vibration of U.S.
Patent No. 2,965,435 can be used.
The relatively brief unhairing step can be followed by the
longer (4 to 16 hours) liming step. The spent unhairing liquors
with the dissolved hair are drained from the hides and a fresh
saturated lime solution is added. The action of lime not only
loosens the hair but opens up the collagen fiber structure.
Collagen swells outside of its isoelectric point in either acid
or base in 8 to 48 hours. This swelling leads to subsequent
fiber separation and allows relatively rapid penetration of the
inorganic pyrophosphate solution of the invention into the raw
hide.
The liming step, when complete, is followed by deliming.
The hide is washed to remove soluble lime and hair particles.
At this point, the stock is at a pH of 12.5. The most widely
used deliming salt is ammonium sulfate, which lowers the pH to 8
to 9.
Puering is the treatment of delimed or partially delimed
skins. Bating is a similar process, generally 'synthetic' bates
are used; these contain enzymes, obtained from the pancreas of
animals, to which neutral deliming salts are added. Puering and
~ating assist in the removal of short hairs, lime soaps, and
cementing substances in the skin, and in depleting and deliming.
As a result of this process, the stretch and pliability of the
leather is increased. Puering and bating are optional in the
process of preparing edible raw hide for dogs and other animals.
The invention product is dried so that it comprises a dry
raw hide strip containing at least one inorganic pyrophosphate.
13~8179
The invention product should be slightly acid to near
neutral.
The invention product is chewable, tough and flexible.
When chewed by dogs, the invention product cleans teeth
surfaces, removes tartar (by mechanical action), and exercises
and massages the gums. The pyrophosphate in the invention
prevents the formation of tartar on the dog's teeth.
The inorganic pyrophosphates are anti-tartar, anti-plaque
or anti-calculus agents. The invention product exhibits
anti-tartar properties over its normal shelf-life. The
invention product does not adversely affect canine tooth enamel.
Hides are normally prefleshed to remove excess flesh before
shipping to companies that prepare raw hide therefrom. If the
hides have been pre-soaked in salt, the salt can be removed by
conventional methods.
Air drying is satisfactory for hides, but it must not be
too slow or putrefaction may begin. If the air drying is too
fast, the outer surface may become hard and dry while the inner
parts still have enough moisture to support bacterial growth.
Fresh hides, if immediately removed from the animal, can be
chilled and washed to remove any excess manure and then sprayed
with a disinfectant. The longer the period of time that the
disinfectant is effective, the longer it will be before there is
any damage to the hides and the greater the distance that the
hides can be shipped. One should make sure that the
disinfectant is removed before or during the dehairing and/or
liming steps.
1~38173
The raw hide is preferably made from cattle hides, but can
be made from horse hides, calf skins, sheep skins, goat skins,
kid skins, marsupial skins, buffalo hides and pig skins, for
example. Fresh cattle hides contain 65 to 70 percent of water,
30 to 35 percent of dry substance, and less than 1 percent of
ash. The dry substance is largely made up of the fibrous
proteins, collagen, keratin, elastin and reticulin. The main
components of the ash, listed in decreasing concentratLon, are
phosphorus, potassium, sodium, arsenic, magnesium and calcium.
Collagen in the hides is responsible for the toughness and
strength in the raw hide.
Liming is a process in which the hides or skins are
immersed in solutions of milk of lime, or slaked lime, to which
small amounts of sodium sulphide, ammonium salts, or sometimes
enzymes may be added. The object of liming is primarily to
loosen the hair, usually by destroying or loosening the
epidermis: at the same time the fibrous structure becomes
swollen and plumped with a partial separation of the fibres.
Lime and other alkalis combine with the natural grease in the
skin to form soaps, which are removed in the subsequent bating
and scudding operations. Liming may be carried out by immersing
~the pelts in pits, paddles, or drums.
In pit liming the hides or skins are placed in brick or
concrete pits. The goods are immersed in lime liquor in the
pits for three days, after which time either the liquor is
strengthened by the addition of freshly slaked lime paste (one
pit system), or the goods are transferred to a once-used lime
liquor and after a further three days placed in a new liquor
1338179
(three pit system), the total period being 8 to 10 days. Pit
liming is laborious as the goods must be hauled frequently from
the pits to permit circulation of the liquor. Mechanical
devices have been devised for agitating lime liquors but have
not met with general acceptance. Instead of using pits, liming
in a drum is more generally favored since it reduces both time
and labor.
Unhairing or dehairing is a process in which the hair is
removed from the skin after it has been loosened by liming.
This may be done manually by means of a blunt-edged knife which
is tilted away from the operator, so that the hair and scud are
pushed or scraped off the skin. Unhairing machines, in which
the hair side of the skins is brought near to a rapidly
revolving cylinder fitted with a series of blunt blades, have
largely superseded hand unhaiting.
Any adipose tissue remaining on the flesh side of the skin
is removed, after liming, in the process of 'fleshing'. A
special knife is used for hand fleshing, but the process is
usually carried out by means of a fleshing machine comprising a
revolving roller fitted with sharp spiral blades.
The deliming is preferably complete. Un~ess the lime is
`removed, the finished leather is hard with a brittle grain and
shows discolorations. Only about 50 percent of the lime can be
removed from the skin by washing in running water, the residual
lime being combined with some of the free acid groups in the
collagen. By treatment with inorganic acids, organic acids, or
acid salts, complete removal of lime is effected.
56
1~38179
The hides, skins, or leather are often separated or split
into two sections or layers of even thickness; the outer or
grain layer, and the under or flesh layer. The splitting is
usually done on a band knife splitting machine.
The prepared raw hides can be cut into strips by a cutter
that exerts a scissor-like action.
The lime treatment apparently opens up the collagen fiber
structure and allows relatively rapid penetration of the
pyrophosphate solution into the raw hide. The pyrophosphate
solution should usually contain only water and the inorganic
pyrophosphate. Water-soluble flavorants, e.g., liver, beef,
cheese, etc., can be included in the pyrophosphate solution.
Depending upon the desired pH of the pyrophosphate solution, an
inorganic base (e.g., NaOH, KOH, CaOH, LioH, MgOH, etc.) or an
inorganic acid (e.g., H2SO4' HCl, etc.) can be used to adjust
the pH. Use of an acid or base has the disadvantage of
resulting in unwanted non-pyrophosphate salts. Preferably the
pH adjustment is done by using ratios of inorganic
pyrophosphates having different pHs. The length of treatment of
the raw hide with the pyrophosphate solution is one
determinative factor in the degree of penetration, that is,
surface, intermediate or completely.
The solvent is preferably water, but other non-toxic,
edible solvents, such as, ethanol or ethanol/water, can be used.
The problem of the necessity of solvent removal from the treated
raw hide due to toxicity is to be avoided in most cases. If a
mixture of ethanol and water is used, the amount of ethanol in
the mixture is generally about 5 to about 60 percent, preferably
13~8179
about 5 to about 25 percent. When one or more of the inor-
ganlc pyrophosphates is not water soluble, lt may be ethanol
soluble.
The invention includes the use of at least one inor-
ganic pyrophosphate. Preferably the inorganic pyrophosphates
are water soluble. A water insoluble pyrophosphate in a
slurry may tend to deposit in the surface regions of the raw
hide. The use of very fine partlcles of a water insoluble
lnorganlc pyrophosphate may provlde better penetratlon lnto
the interior regions of the raw hide. Water insoluble inor-
ganic pyrophosphates have abrasive actlon.
The inorganic pyrophosphates are preferably alkali
metal pyrophosphates. The preferred alkali metal pyrophos-
phates are tetrasodium pyrophosphate and tetrapotassium pyro-
phosphate. An example of a useful tetraalkali metal pyrophos-
phate is tetralithium pyrophosphate. Alkaline earth metal
pyrophosphates are also useful, but they are generally insol-
uble ln water. Preferably the lnorganic pyrophosphates are
soluble in water.
Kirk & Othmer, "Encyclopedia Of Chemical Technology",
2nd Ed., Vol. 15, (1965), pages 232 to 276, discloses a number
of water-soluble and water insoluble inorganlc pyrophosphate
salts.
Mn+2PnO3n+l, where M is a univalent
metal, is the formula for univalent metal pyrophosphates when
n is 2. The formula M'nPnO3n+1, where M' is a divalent metal,
is the formula for divalent metal pyrophosphates when n is 2.
Such univalent metal pyrophosphates and divalent metal pyro-
phosphates can be
- 58 -
D 73783-60
133817~
used in the invention. Polypyrophosphates have the formula
Mn+2PnO3n+1 or M ~ nPn3n+1' there n is 2,3,4,5..., and the oxide
ratio R between the cationic oxides (M20) iand M ~ O and anionic
oxides (P205) is between 1 and 2. The oxide ratio for
pyrophosphate is 2.
Examples of dialkaline metal pyrophosphates are dicalcium
pyrophosphate, dibarium pyrophosphate and dimagnesium
pyrophosphate. Trialkali metal monoacid pyrophosphates, such
as, trisodium hydrogen pyrophosphate, can be used. Monoalkali
metal triacid pyrophosphates, such as, sodium trihydrogen
pyrophosphate, can also be present in limited amounts. Examples
of other inorganic pyrophosphates include dimanganese
pyrophosphate and dizinc pyrophosphate.
Tetrasodium pyrophosphate, one part, is soluble in 13 parts
of cold water and in 2.5 parts of boiling water. It is
insoluble in ethanol. Dicalcium pyrophosphate is practically
insoluble in water. The invention use of the term "solution"
includes slurries, suspensions and the like. Tetrapotassium
pyrophosphate is freely soluble in water and is insoluble in
ethanol.
The solution can also contain suitable s~rfactants or
emulsifying agents. The emulsifier is best only used in minor
amounts which are effective in keeping a water insoluble
inorganic pyrophosphate in suspension.
The invention product does not include any
fluorine-containing compound or other fluoride ion source, or
quaternary ammonium compounds. The invention does not include
organic acid pyrophosphates.
59
13~8l7~
Preferably a mixture of trisodium monoacid pyrophosphate
and tetrapotassium pyrophosphate is used (in a ratio to achieve
the desired pH).
Federal GRAS regulations are that the upper amount of
pyrophosphate moiety, P2O7' delivered is 0.5 weight percent
(based on the total composition). The maximum allowable GRAS
level in a composition for sodium acid pyrophosphate (SAPP) is
0.3 weight percent and tetrasodium pyrophosphate (TSPP) is 0.5
weight percent, such weight percentages being based on the total
weight of the product. If GRAS levels change (rise) or if
higher levels are allowed by the regulatory agencies, higher
levels can be used in the invention.
The preferred invention solution contains trisodium
monoacid pyrophosphate (SAPP) and tetrapotassium pyrophosphate
in a weight ratio of about 60 to about 40.
The pyrophosphate(s) is used in sufficient amount to
deliver generally from about 0.1 to about 5 weight percent,
preferably from 0.4 to 0.5 weight percent (based on the total
composition), of P2O7.
A study of the application of aqueous solutions of a
mixture of tetrasodium pyrophosphate and sodium acid
pyrophosphate to the teeth of dogs by spraying for one month
resulted in dose response data. The aqueous solutions
containing 5 and 3 weight percent of such pyrophosphate mixture
resulted in significant reductions in tartar accumulation. The
aqueous solutions containing 1.5 and 0.5 weight percent of such
pyrophosphate mixture resulted in directional trends of
reductions in tartar accumulation.
133817~
The ratio of sodium acid pyrophosphate (SAPP) to
tetrapotassium pyrophosphates (TKPP) is between 0.01 to 99.99
and 99.99 to 0.01 weight percent.
The pH of the solution of at least one inorganic
pyrophosphate compound (salt) is generally in the range of about
4 to about 10.5, typically from about 5 to about 8, preferably
from about 5.5 to about 6.5, most preferably about 6.
The solution application usually is conducted at a
temperature of about 45 to about 140F, preferably about 60 to
about 110F.
The solution containing the pyrophosphate compound-is
allowed to fully penetrate the raw hide or to penetrate only the
surface region of the raw hide. The raw hide is in the uncut
form or preferably is in strip form.
The solution can be applied to the raw hide by any suitable
means, such as, spraying, soaking in a container, etc., but the
preferred method is by dipping the raw hide strips in the
solution. (The raw hide strips can be in long rope form; the
coating applied and dried; and the rope then cut into shorter
strips.)
After treating the raw hide with the pyrophosphate
compound, the raw hide is dried. While the treated raw hide is
preferably air dried, it is also advantageous to dry the treated
raw hide using applied heat, e.g., in a hot air oven (at a
temperature of say 75 to 300F).
The invention product can be raw hide in any shape which
can be chewed by dogs. Examples of such raw hide shapes are
strips, balls made up of pieces or strips, knotted strips, bones
1338173
made up of pieces of strips, curled pieces, etc. The raw hide
can be that which has been molded (e.g., compressed, extruded,
stamped, tabletted, etc.) and formed.
The invention deals primarily with dogs, but has a scope of
teeth bearing non-human animals or mammals, such as, cats. The
invention composition is used to reduce or prevent tartar
accumulation on canine teeth and other non-human animal or
mammal teeth.
The invention also includes a process for preparing raw
hide having a coating containing at least one inorganic
pyrophosphate compound, comprising:
(a) subjecting raw hide to a liquefied coating material at
least one inorganic pyrophosphate compound; thereby, forming a
coating of such liquefied coating material on the raw hide; and
(b) drying the raw hide having a coating containing said at
least one inorganic pyrophosphate compound.
The invention further includes raw hide having a coating
containing at least one inorganic pyrophosphate salt. The
invention also include a process for the prevention of tartar
accumulation on the teeth of dogs comprising chewing and/or
eating the raw hide having a coating containing at least one
~norganic pyrophosphate.
The above information on the preparation of raw hide is
applicable here.
When the invention liquefied coating material is applied to
the raw hide, its consistency, viscosity, solids content, etc.,
keeps it primarily on the surface of the raw hide. Some of the
liquefied coating material will seep into the surface regions of
1338173
the raw hide, thereby, helping to anchor or adhere the coating
to the raw hide once it is dried.
The invention product is dried so that it comprises a dry
raw hide strip having at least one inorganic pyrophosphate.
Dogs prefer the coated product over uncoated raw hide,
apparently are an individual dogs' preference. Dogs appear to
attempt to gnaw the coating off of the coated raw hide after the
initial smell and taste. After the coating is gone sometimes
the raw hide is left uneaten. The invention product is very
effective in reducing the accumulation of tartar on the teeth of
dogs.
The invention product should be slightly acid to near
neutral.
The invention product is chewable, tough and flexible.
When chewed by dogs, the invention product cleans teeth
surfaces, removes tartar (by mechanical action), and exercises
and massages the gums. The pyrophosphate in the invention
prevents the formation of tartar on the dog's teeth.
The inorganic pyrophosphates are anti-tartar, anti-plaque
or anti-calculus agents. The invention product exhibits
anti-tartar properties over its normal shelf-iife.
The invention further includes a coating comprised of
malto-dextrin, food starch or modified food starch, optional
colorant, optional flavorant for animals or humans suitable
polysaccharide gum (preferably xanthan gum), surfactant
(preferably lecithin or modified lecithin), vegetable fat or
animal fat). The coating can be used on baked dough.
63
1338179
The raw hide is preferably made from cattle hides, but can
be made from horse hides, calf skins, sheep skins, goat skins,
kid skins, marsupial skins, buffalo hides and pig skins, for
example. Fresh cattle hides contain 65 to 70 percent of water,
30 to 35 percent of dry substance, and less than 1 percent of
ash. The dry substance is largely made up of the fibrous
proteins, collagen, keratin, elastin, and reticulin. The main
components of the ash, listed in decreasing concentration, are
phosphorus, potassium, sodium, arsenic, magnesium, and calcium.
Collagen in the hides is responsible for the toughness and
strength in the raw hide.
The deliming is preferably complete. Unless the lime is
removed, the finished leather is hard with a brittle grain and
shows discolorations. Only about 50 percent of the lime can be
removed from the skin by washing in running water, the residual
lime being combined with some of the free acid groups in the
collagen. By treatment with inorganic acids, organic acids, or
acid salts complete removal of lime is effected.
The hides, skins, or leather are often separated or split
into two sections or layers of even thickness; the outer or
grain layer, and the under or flesh layer. Tfie splitting is
usually done on a band knife splitting machine.
The prepared raw hides can be cut into strips by a cutter
that exerts a scissor-like action.
The solvent used in the coating is preferably water, but
other non-toxic, edible solvents, such as, ethanol or
ethanol/water, can be used. The problem of the necessity of
solvent removal from the treated raw hide due to toxicity is to
64
1~3817~
be avolded ln most cases. If a mlxture of ethanol and water
ls used, the amount of ethanol ln the mlxture ls generally
about 5 to about 60 percent, preferably about 5 to about 25
percent. When one or more of the lnorganlc pyrophosphates ls
not water soluble, lt may be ethanol soluble.
The invention lncludes the use of at least one lnor-
ganic pyrophosphate. Preferably the lnorganlc pyrophosphates
are water soluble. A water insoluble lnorganlc pyrophos-
phate(s) can be used by ltself or ln a mlxture wlth at least
one water soluble lnorganlc pyrophosphate. Water lnsoluble
lngredlents result ln a slurry. The use of very flne par-
tlcles of a water lnsoluble lnorganlc pyrophosphate provides
better suspenslon ln the coatlng formulatlon. Water insoluble
lnorganlc pyrophosphates have abraslve actlon.
The lnorganlc pyrophosphates are preferably alkall
metal pyrophosphates. The preferred alkali metal pyrophos-
phates are tetrasodlum pyrophosphate and tetrapotasslum
pyrophosphate. An example of a useful tetraalkall metal
pyrophosphate ls tetralithlum pyrophosphate. Alkallne earth
metal pyrophosphates are also useful, but they are generally
lnsoluble ln water. Preferably the lnorganlc pyrophosphates
are soluble ln water.
Kirk & Othmer, "Encyclopedla Of Chemlcal Technology",
2nd Ed., Vol. 15, (1965), page 232 to 276, dlscloses a number
of water-soluble and water lnsoluble lnorganlc pyrophosphate
salts.
- 65 -
73783-60
1338179
Examples of dialkaline metal pyrophosphates are dicalcium
pyrophosphate, dibarium pyrophosphate, and (dimagnesium
pyrophosphate. Trialkali metal monoacid pyrophosphates, such
as, trisodium hydrogen pyrophosphate, can be used. Monoalkali
metal triacid pyrophosphates, such as, sodium trihydrogen
pyrophosphate, can also be present in limited amounts. Examples
of other inorganic pyrophosphates include dimanganese
pyrophosphate and dizinc pyrophosphate.
The formula Mn+2PnO3n+1l where M is a univalent metal, is the
formula for univalent metal pyrophosphates when n is 2. The
formula M'nPnO3n+,, where M' is a divalent metal, is the formula
for divalent metal pyrophosphates when n is 2. Such univalent
metal pyrophosphates and divalent metal pyrophosphates can be
used in the invention. Polyphosphates have the formula
Mn+2PnO3n+1' or M~nPnO3n+1' where n is 2,3,4,5,..., and the oxide
ratio R between the cationic oxides and anionic oxides (P205) is
between 1 and 2. The oxide ratio for pyrophosphate is 2.
Tetrasodium pyrophosphate, one part, is soluble in 13 parts
of cold water and in 2.5 parts of boiling water. It is
insoluble in ethanol. Dicalcium pyrophosphate is practically
insoluble in water. The invention use of the term "solution"
includes slurries, suspensions and the like. Tetrapotassium
pyrophosphate is freely soluble in water and is insoluble in
ethanol.
The invention product does not include any
fluorine-containing compound or other fluoride ion source, or
quaternary ammonium compounds. The invention does not include
organic acid pyrophosphates.
66
1~38173
Preferably a mixture of trisodium monoacid pyrophosphate
and tetrapotassium pyrophosphate is used (in a ratio to achieve
the desired pH).
Federal GRAS regulations are that the upper amount of
pyrophosphate moiety, P207, delivered is 0.5 weight percent
(based on the total composition). The maximum allowable GRAS
level in a composition for sodium acid pyrophosphate (SAPP) is
0.3 weight percent and tetrasodium pyrophosphate (TSPP) is 0.5
weight percent, such weight percentages being based on the total
weight of the product.
The preferred invention solution contains trisodium
monoacid pyrophosphate (SAPP) and tetrapotassium pyrophosphate
in a weight ratio of about 60 to about 40.
The pyrophosphate(s) is used in sufficient amount to
deliver generally from about 0.1 to about 5, preferably from 0.4
to 0.5 weight percent (based on the total composition) of P207.
A study of the application of aqueous solutions of a
mixture of tetrasodium pyrophosphate and sodium acid
pyrophosphate to the teeth of dogs by spraying for one month
resulted in does response data. The aqueous solutions
containing 5 and 3 weight percent of such pyrophosphate mixture
~esulted in significant reduction sin tartar accumulation. The
aqueous solutions containing 1.5 and 0.5 weight percent resulted
of such pyrophosphate mixture in directional trends of
reductions in tartar accumulation.
The ratio of sodium acid pyrophosphate (SAPP) to
tetrapotassium pyrophosphate (TKPP) is between 0.01 to 99.99
weight percent and 99.99 to 0.01 weight percent.
67
13~817~
The pH of the solution of at least one inorganic
pyrophosphate compound (salt) is generally in the range of about
4 to about 10.5, typically from about 5 to about 8, preferably
from about 5.5 to about 6.5, most preferably about 6.
The solution application is usually conducted at a
temperature of about 45 to about 200F, preferably about 60 to
about 190F.
The solution can also contain suitable surfactants or
emulsifying agents. The preferred surfactant is lecithin or a
modified lecithin, most preferably a modified lecithin which is
in a dry form. Preferably about 0.5 to about 1.75 weight
percent of the lecithin or modified lecithin is used. The
surfactant or wetting agent helps the coating material to apply
over the entire surface of the raw hide strips.
The liquefied coating formulation best contains at least
one suspension agent. The preferred suspension agent is a
polysaccharide gum. Preferably about 0.05 to 1.25 weight
percent of xanthan gum is used. Xanthan gum is one of the few
gums which acts as an acceptable suspension agent in the
invention. Other suitable gums and mucilages can be used.
Xanthan gum is preferred because it is stable over a broad range
of temperature and holds the same viscosity in the liquefied
coating formulation over the broad temperature range. The
xanthan gum has a bodying effect so that little or no separation
occurs.
Malto-dextrin produced by hydrolyzing corn starch is
preferred. It serves as a carrier (bodying), binding agent and
68
1:~38179
suspension agent and helps the appearance of the coating. Other
malto-dextrins can also be used for the same functions.
An adhesive or binding agent, such as, malto-dextrins, is
needed in the coating slurry to help the coating material bind
(adhere) to the raw hide when the raw hide is dipped in the
coating slurry. Preferably about 5 to about 15 weight percent
of the malto-dextrin is included in the coating material.
A carrier, such as, starch or a modified food starch, is
included in the coating formulation. Preferably about 0.1 to
about 5 weight percent of the food starch or modified food
starch is included in the coating material. The food starch or
modified food starch also serves to control the viscosity.
Animal fat preferably is included for flavor purposes.
Other suitable flavorants can be included, particularly salt.
The flavorants can be any dairy product flavorant, such as, milk
or cheese, meat flavorants, such as, liver or beef, poultry and
fish. Flavorants help provide palatability for the invention
coating.
Preferably a hydrogenated vegetable oil, is included in the
coating formulation for sheen and to modify the melting point of
the formula fats in the finished product. It also helps to
prevent flaking of the coating; also the coating does not have a
tacky feeling.
Any suitable colorant can be included in the coating
formulation. The preferred colorant is caramel color, which
also provides some flavor to the product.
The coating also incorporates sufficient water to achieve
the liquefied coating composition. Amounts of other ingredients
69
133~17~
are those which are effective to achieve their functions in the
coating formulation.
The preferred coating formulation, besides the inorganic
pyrophosphates, contains animal fat, a surfactant, such as, a
modified lethicin, polysaccharide gum, a modified food starch,
flavorant, colorant, hydrogenated vegetable oil, and a carrier,
such as malto-dextrin and water.
The coating formulation should be viscous enough so that
the coating formulation generally only coats the surface regions
of the raw hide. The presence of coating in the surface regions
of the raw hide helps to anchor the resultant coating and to
prevent the coating from easily being separated from the raw
hide during handling and shipping and the coating is strictly a
surface phenomena on the raw hide.
The coating slurry can be applied to the raw hide by any
suitable means, such as, spraying, soaking in a container, etc.,
but the preferred method is by dipping the raw hide strips in
the solution. (The raw hide could be in long rope into shorter
strips.) The coating slurry is applied generally at a
temperature of 45 to 200F, preferably at about 60 to about
190F, and most preferably at about 180. The coating slurry
~as a low microbial profile at such higher temperatures.
After treating the raw hide with the pyrophosphate compound
slurry, the raw hide is dried. While the treated raw hide is
preferably air dried, it is also advantageous to air oven (at a
temperature of say 75 to 300F).
The invention product can be raw hide in any shape which
can be chewed by dogs. Examples of such raw hide shapes are
133~17~
strips, balls made up of pieces or strips, knotted strips, bones
made up of pieces or strips, curled pieces, etc. The raw hide
can be that which has been molded (e.g., compressed, extruded,
stamped, tabletted, etc.) and formed.
The invention deals primarily with dogs, but has a scope of
teeth bearing non-human animals or mammals, such as, cats. The
invention composition is used to reduce or prevent tartar
accumulation on canine teeth and other non-human animal or
mammal teeth.
1338179
The preferred coating formulation is:
Table 3
Ingredients Percentages
Specific Ranges
Sodium acid pyrophosphate (SAPP),
anhydrous powder, (non-leavening
type) 1.73 0.25 to 5
Tetrapotassium pyrophosphate
(TKPP), anhydrous powder 1.15 0.25 to 5
Salt 0.50 0.05 to 2.5
Malto-Dextrin 9.17 2 to 30
Modified Food Starch 2.00 0.1 to 10
Colorant 0.50 0.01 to 3
Flavorant 2.00 0.01 to 5
Xanthan 0.20 0.05 to 1.5
Lecithin or Modified Lecithin1.25 0.5 to 1.75
Vegetable Fat 0.50 0.1 to 3
Animal Fat 1.00 0.1 to 5
Subtotal20.00
Water 80.00 50 to 97
Total 100.00
133817~
The invention includes a viscous, liquefied coating
formulation comprised of a surfactant, an effective polysaccharide
gum, a binding agent, a starch carrier, a hydrogenated vegetable
oil. A preferred coating formulation contains a surfactant, such
as, lecithin or modified lecithin, xanthan gum (or other suitable
polysaccharide gum), a starch or modified food starch,
hydrogenated vegetable oil and a binding agent, such as,
malto-dextrin, and water. Optional ingredients humectant,
preferably propylene glycol, can be used in the coating
formulation. The invention coating can, but does not have to,
contain at least one inorganic pyrophosphate salt.
The invention coating can be applied to any suitable human or
animal food, such as, non-human animals, e.g., cats and dogs. The
invention coating is preferably applied to baked dog biscuits and
then both are dried.
The liquefied coating formulation best contains at least one
suspension agent. The preferred suspension agent is a
polysaccharide gum, most preferably xanthan gum. Preferably about
0.05 to 1.25 weight percent of polysacchaEide gum (xanthan gum) is
used. Xanthan gum is one of the few gums which acts as an
acceptable suspension agent in the invention.' The xanthan gum is
"an excellent agent for controlling the bodying effect, as it is
stable over a broad temperature range, i.e., it holds the same
viscosity over a large temperature range without any separation of
the coating ingredients. Other suitable gums and mucilages can be
used.
Malto-dextrin produced by hydrolyzing corn starch is
preferred: it serves as a carrier (bodying), binding agent and
1338179
suspension agent and helps the appearance of the coating; and it
is a preferred ingredient. Other malto-dextrins can also be used.
An adhesive or binding agent, such as, malto-dextrins, is
needed in the coating slurry to help the coating material bind
(adhere) to the raw hide when the raw hide is dipped in the
coating slurry. Preferably about 5 to about 15 weight percent of
the malto-dextrin is included in the coating material.
A carrier, such as, starch or a modified food starch, is
included in the coating formulation. Preferably about 0.1 to
about 5 weight percent of the food starch or modified food starch
is included in the coating material. The food starch or modified
food starch also serves to control the viscosity.
Animal fat preferably is included for flavor purposes.
Other suitable flavorants can be used or included,
particularly salt. The flavorants can be any dairy product
flavorant, such as milk or cheese, meat flavorants, such as, liver
or beef, poultry and fish. Flavorants help provide palatability
for the invention coating.
Preferably a hydrogenated vegetable oil is included in the
coating formulation for sheen and to modify the melting point of
the formula fats in the finished product. It also helps to
prevent flaking of the coating; also the coating does not have a
tacky feeling.
Any suitable colorant can be included in the coating
formulation. The preferred is caramel color which also provides
some flavor to the product.
The coating also incorporates sufficient water to achieve the
liquefied coating composition. Amounts of the other ingredients
1~38173
are those which are effective to achleve thelr functlons in
the coatlng formulatlon.
A preferred coatlng formulatlon for dog blscults
contaln water, anlmal fat, a surfactant, such as, a modifled
leclthln, xanthan gum, a modlfled food starch, flavorant,
colorant, hydrogenated vegetable oll and a carrler, such as a
malto-dextrln.
Another preferred embodiment for the invention coat-
ing for dog blscults and ranges of the lngredlents of the
coating is:
Percentages
Inqredients Specific Ranqes
Salt 0.50 0.05 to 2.5
Malto-Dextrin 9.17 2 to 30
Modlfled Food Starch 2.00 0.1 to 10
Colorant 0.50 0.01 to 3
Flavorant 2.00 0.01 to 5
Xanthan 0.20 0.05 to 1.5
Leclthin or Modlfled Leclthln 1.25 0.5 to 1.75
Vegetable Fat 0.50 0.1 to 3
Anlmal Fat 1.00 0.1 to 5
Subtotal 20.00
Water 80.00 50 to 97
Total 100.00
The lnventlon coating formulation can contain a
humectant, such as, corn syrup, sugar and polyalcohols, such
as, propylene glycol (preferred), sorbitol and glycerin.
The lnvention product does not lnclude any fluorlne
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contalnlng compound or other fluorlde lon source, or
guaternary ammonlum compounds.
The lnventlon coatlng can be applled, for example, to
any sultable dog food, such as, dog blscuits, whlch can be
made from any sultable dough comprlslng at least flour, meal,
fat and water can be employed for the product. For lnstance,
when the deslred product ls a canine biscult, a conventlonal
dough for dog blscults can be used, optlonally contalnlng
dlscrete partlcles of meat and/or meat byproducts or farlna-
ceous material. Such doughs typcially contain fat solids.Examples of suitable doughs for the production of hard dog
blscults are disclosed in U.S. Patent No. 4,454,163, and
sultable doughs for the productlon of soft dog blscults (con-
talnlng humectant to control water actlvlty) are dlsclosed ln
U.S. Patent No. 4,454,164. Partlculate protelnaceous par-
tlcles, such as partlcles of meat, texturlzed vegetable pro-
teln and/or meat byproducts can be lncorporated to add flavor
to the blscults and texturlze the surface. Partlculate farl-
naceous materlals such as bran partlcles can also be employed
to te~turize the lnterlor and/or surface of the blscults and
to provlde other useful propertles to the product. A dough
found to produce blscults hlghly palatable to dogs lncludes
suitable proportlons of wheat flour, wheat meal, soybean meal,
meat and bone meal, anlmal fat and natural flavors ln admlx-
ture wlth water. The meal used ln the doughs sultable for
productlon of blscults useful ln the lnventlon can comprlse
meat and/or bone and/or vegetable matter lncludlng farlnaceous
materlals, materlals prepared from legumes such as bean and
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peas, tuberous materlals such as potato meal, and the like.
The meals can be finely or coarsely ground as desired for the
texture. Flours made from any suitable farinaceous material
can be used.
The doughs generally have a water actlvity of about
0.90 and above upon completlon of mixing of the dough lngredi-
ents. A suitable dough contalns farlnaceous materlal, an
edlble oil, an antioxidant, an antimycotlc, salt, animal fat,
added vltamlns and minerals, such as those disclosed in U.S.
Patent No. 4,229,485, column 5, llnes 7 to 57.
The composltlons of the lnventlon also preferably
contain at least one animal-derived proteinaceous meal such as
meat meal, bone meal and fish meal. A good biscuit dough for
producing the biscuits of the inventlon contalns about 50 to
60 percent by weight of wheat flour, about 5 to 10 percent by
welght of soybean meal, about 3 to 10 percent by welght of
meat meal and bone meal, about 1 to 5 percent of wheat meal,
about 1 to 5 percent of anlmal fat preserved wlth BHA, about
20 to 30 percent by weight of water, and about 2 to 5 percent
by weight of natural flavors, vitamln and mineral preblend,
and acldulant.
The dog blscult doughs can contaln a softenlng agent.
Any sultable softenlng agent can be used. The preferred
humectant ls propylene glycol. Examples of other sultable
humectants are corn syrup, sugar and polyalcohols, such as,
sorbitol and glycerin. Any suitable humectant known ln the
art can be used.
The dough ingredlents are generally mlxed at a tem-
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perature of about 45 to about 140F, preferably about 60 to
about 125F.
The dog biscult dough for the outer portlon and the
lnner portion can be mlxed uslng any sultable or conventlonal
equlpment. For example, the mlxlng can be at 20 to 100 rpm.
For example, a
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dry blending step can be done typically at room temperature for a
period of time of about 3 minutes to about 20 minutes. The
dry-blended mixture can then be mixed with the hot water to form a
first stage dough. The water which can be admixed with the
dry-blended mixture is typically at a temperature of about 65 to
about 150F. The hot water can be added, with mixing, over a
period of time of about 3 minutes to about 6 minutes to form the
first stage dough. Then, the fat portion of the biscuit dough can
be admixed with the first stage dough to form the final stage
dough. The fat portion can be added at a temperature at which it
is at least fluid, typically at about 100 to about 150F. The
fat portion can be mixed for a period of time which is sufficient
to form a dough whose homogeneity is visually apparent. A
typically final mixing time is about 3 to about 5 minutes.
Preparation of the dough is achieved at about atmospheric
pressure with mixing of the components being conveniently achieved
in an upright sigma blade mixer or othef bakery-type mixers. The
various ingredients can be added over a period of time or in a
one-shot manner according to the above order of addition.
However, melted fat and water can be added simultaneously and
mixed for 6 to 10 minutes.
The dough can be formed into dough pieces using any suitable
or conventional manner, such as, by extrusion, molding, stamping
or cutting. Any suitable dog biscuit shapes can be used, such as,
bone-shaped canine biscuts. Holes can be formed in the dog
biscuits to facilitate the escape of moisture during baking,
cooking and/or drying.
1338179
The dog biscuit dough pieces can be baked using any suitable
biscuit dough pieces can be passed into an oven such as a
conventional band oven where the biscuits are baked. The conveyor
belts of the oven can be coated with an edible lubricant such as a
natural or synthetic cooking oil or shortening to facilitate
separation from the conveyor belts of the baked products.
Temperatures in the range of about 300 to about 600F can be
used.
The invention coating can be applied to the dog biscuit dough
pieces before baking followed by baking at a low baking
temperature of, say, about 300 to about 310F. It is preferable
to apply the invention coating after the dog biscuit dough pieces
have been baked.
The baked dog biscuits can also be subjected to subsequent
drying at temperatures of about 200 to 400F (e.g., for 25 to 12
mintues), either within the baking oven or separately, to produce
the desired moisture content. If dealing with coating dog
biscuits which have been baked with the coating on the dog
@iscuits, the baked, coated dog biscuits should not be dried at a
temperature at above about 300F. Drying is usually done at a
temperature of about 75 to 300F. to achieve the desired
`moistute content (about 5 to 13 weight percent).
The invention coating is preferably applied to baked dog
biscuits. The coating is preferably applied to the baked dog
biscuits in the form of a liquefied coating formulation by any
encompass all or part of the baked dog biscuits.
The coating formulation usually is viscous enough so that the
coating formulation generally only coats the surface regions of
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the baked dog biscuits. The presence of coating in the sutface
regions of the baked dog biscuits helps to anchor the resultant
coating and to prevent the coating from easily being shipping.
The coating slurry can be applid to the baked dog biscuits by
any suitable maens, such as, spraying, dipping, etc. The coating
slurry is applied generally at a temperature of 45 to 200F,
preferably at about 60 to about 190F, and most preferably at
about 180F, (the baked dog biscuits best having been cooled, of
allowed to cool, to less than 200F). The coating slurry has a
low microbial profile at such higher temperatures.
After treating the baked dog biscuits with the invention
coating slurry, the coated baked dog biscuits are dried. While
the coated, baked dog biscuits are preferably air dired, it is
also advantageous to dry the coated animal food using applied
heat, e.g., in a hot air oven at a temperature of say 75 to 300F
(typically 250F for 20 minutes). The coated dog biscuits of 0.70
or less. On a weight basis, the moisture content of the final
coated biscuit product is less than or equal to about 15 percent
by weight and preferably about 10 to 12 percent by weight of the
final biscuit at 70 percent relative humidity. The coated dog
biscuits are shelf stable.
The animal food within the scope of this invention needs to
have a sufficient integrity to not fall apart during processing
and handling, especially, so that the coating can be applied,
dried/baked, etc., without losing its integrity or cracking. The
animal food is best in the form of pieces or the like, such as,
kibbles, biscuits, snacks, etc. The animal food pieces can be
made by any suitable forming means, such as, extruding, molding,
1338179
stamplng, etc. The invention composition is used to reduce
and control tartar accumulation on canlne teeth.
The animal food can be the dog food disclosed in
commonly-owned, U.S. Patent No. 4,904,494, flled on
September 9, 1988, entitled "Chewy Dog Snacks". A chewy,
seml-plastlc, non-extruded, non-porous, microblologically-
stable dog food which includes 12 to about 30 weight percent,
based upon the total weight of the dog food, of gelatin; at
least one acidulant; at least one cereal starch-contalnlng
textural agent; at least one release agent; at least one taste
agent; at least one sugar; salt; and added water. The dog
food ls in a molded form. The dog food has a pH of about 3 to
5, and has a moisture content of about 10 to 25 weight per-
cent, based on the welght of the dog food. The process for
preparing the dog food lncludes (a) mixing the dry components
and liquid components with low speed agltatlon and contlnulng
the mlxlng untll a dough ls obtained; (b) forming the dough by
molding or rotary moldlng into molded snack or biscuit; (c)
conditioning the molded dough at 185 to 200F for about 7 to
8 minutes; and (d) packaglng the molded dog snack or blscuit
in a protective package.
The invention also involves an anlmal or dog food,
such as, a dog blscuit, having a soft, edible center whlch
contalns at least one inorganic pyrophosphate. The center ls
made soft by the lnclusion of a softening agent, such as, at
least one humectant. The preferred humectant ls propylene
glycol. The animal food reduces or prevents the accumulatlon
of tartar on the animal's teeth.
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The invention also involves animal foods, such as, dog foods,
having a coating containing at least an inorganic pyrophosphate.
The coated animal food reduces or prevents the accumulation of
tartar on the animal's teeth.
The invention also involves swabs, gauze and other like
materials having absorbed/adsorbed therein and/or thereon a
solution containing at least one inorganic pyrophosphate. The
treated swab or treated gauze reduces or prevents the accumulation
of tartar on the animal's teeth.
The invention further involves swabs, gauze or other like
materials having thereon and/or therein a coating containing at
least one inorganic pyrophosphate. The coated swab or coated
gauze reduces or prevents the accumulation of tartar on the
animal's teeth.
The invention involves meat jerky, such as, beef jerky,
having absorbed/adsorbed therein and/or thereon a solution
containing at least one inorganic pyrophosphate. The treated meat
jerky reduces or prevents the accumulation of tartar on the
animal's teeth.
The invention involves meat jerky, such as, beef jerky,
having a coating therein and/or thereon a coating containing at
least one inorganic pyrophosphate. The treated meat jerky reduces
or prevents or reduces the accumulation of tartar on the animal's
teeth.
The invention still further involves a process of preventing
or reducing tartar accumulation on the teeth of an animal,
comprising:
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1338179
(a) spraying an aqueous solutlon containlng at least
one lnorganlc pyrophosphate onto an anlmal food; and
(b) havlng an anlmal consume the treated anlmal
food.
The lnventlon deals prlmarlly wlth dogs, but has a
scope of teeth bearlng non-human mammals and other anlmals,
such as, cats and dogs.
The lnventlon lnvolves a dog food, such as, dog
blscuits, havlng a soft center contalnlng at least one lnor-
ganlc pyrophosphate. The center ls softer than the rest ofthe dog blscult, whlch can be a soft or hard dog blscult. The
center ls made soft by the lncluslon of at least one softenlng
agent, such as, at least one humectant.
The outer portlon of the dog food, such as, dog
blscults, can be made from any sultable dog food dough, such
as, sultable dog blscult dough. Any suitable dough comprising
at least one flour, meal, fat and water can be employed for
the product. For instance, when the desired product is a
canlne blscult, a conventlonal dough for dog blscults can be
used, optlonally contalnlng dlscrete particles of meat and/or
meat byproducts or farinaceous material. Such doughs typical-
ly contain fat solids. Examples of suitable doughs for the
production of hard dog biscuits are disclosed in U.S. Patent
No. 4,454,163, and sultable doughs for the productlon of soft
dog biscuits (containlng humectant to control water actlvity)
are dlsclosed in U.S. Patent No. 4,454,164. Particulate
protelnaceous particles, such as particles of meat, texturized
vegetable protein and/or meat byproducts can be incorporated
to add flavor to the biscuits and texturize the surface.
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Particulate farinaceous materials such as bran particles can
also be employed to texturlze the interior and/or surface of
the biscuits and to provide other useful properties to the
product. A dough found to produce biscuits highly palatable
to dogs includes suitable proportions of wheat flour, wheat
meal, soybean meal, meat and bone meal, animal fat and natural
flavors in admixture with water. The meal used in the doughs
suitable for productlon of blscuits useful in the lnventlon
can comprise meat and/or bone and/or vegetable matter includ-
ing farinaceous materlals, materlals prepared from legumes
such as beans and peas, tuberous materials such as potato
meal, and the llke. The meals can be flnely or coarsely
ground as desired for the texture. Flours made from any suit-
able farinaceous material can be used.
The doughs generally have a water actlvlty of about
0.90 and above upon completlon of mlxlng of the dough lngredl-
ents. A sultable dough contalns farlnaceous material, an
edible oil, an antloxldant, an antimycotic, salt, anlmal fat,
added vltamins and minerals, such as those disclosed in U.S.
Patent No. 4,229,485, column 5, llnes 7 to 57.
The composltlons of the invention also preferably
contain at least one animal-derived proteinaceous meal such as
meat meal, bone meal and fish meal. A good blscuit dough for
produclng the blscuits of the invention contalns about 50 to
60 percent by weight wheat flour, about 5 to 10 percent by
welght soybean meal, about 3 to 10 percent by welght meat and
bone meal, about 1 to 5 percent wheat meal, about 1 to 5
percent anlmal fat preserved wlth BHA, about 20 to 30 percent
by weight water, and
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about 2 to 5 percent by weight of natural flavors, vitamin and
mineral preblend, and acidulant.
The soft center portion of the dog biscuit contains a
softening agent if it is made from a dog biscuit dough. Any
suitable softening agent can be used. The preferred humectant is
propylene glycol. Examples of other suitable humectants are corn
syrup, sugar and polyalcohols, such as, sorbitol and glycerin.
Any suitable humectant known in the art can be used.
If the softening agent is used in the outer portion of the
dog biscuit, more of a softening agent should be used in the
central portion to make it softer than the outer portion.
The solvent used in preparing the dog biscuit dough for the
center portion is most preferably water, but other non-toxic,
edible solvents, such as, ethanol or ethanol/water, can be used.
The problem of the necessityof solvent removal from the dough due
to toxicity is to be avoided. If a mixture of ethanol and water
is used, the amount of ethanol in the mixture is generally about 5
to 60 percent, preferably about 5 to about 25 percent. when one
or more of the inorganic pyrophosphates is not water soluble, it
may be ethanol soluble. It may be necessary to use a non-aqueous
solvent, or mixture of water therewith, to incorporate the
`inorganic pyrophosphate.
The invention includes the use of at least one inorganic
pyrophosphate. Preferably the inorganic Pyrophosphate(s) is water
soluble. A mixture of pyrophosphates can be used to provide a
desired pH. Water-insoluble or difficulty soluble inorganic
pyrophosphates can be used.
1338179
The pH of the dough can be adiusted uslng an inor-
ganlc base (e.g., KOH, NaOH, CaOH, LiOH, MgOH, etc.) or an
inorganic base (e.g., H2SO4 HCl, etc.), but this approach has
the disadvantages of possibly causlng a mlsbalance or
overabundance of one or more chemical entities and posslbly
lntroduclng unwanted salts.
Generally 0.1 to 10 weight percent, preferably about
0.5 to about 3.5 weight percent and most preferably about 1.4
to about 2.5 weight percent of inorganic pyrophosphate is
used.
When a mixture of tetrasodium pyrophosphate (TSPP)
and sodium acid pyrophosphate ln aqueous solutlon at the 5
welght percent level was incorporated in dog biscuit dough,
there was reduced dough gluten development, the dog blscuits
were bleached (whitish) and crumbly, and the dog blscuits were
softer (a hardness problem) than the control dog biscuits. At
the level of 3 weight percent of a mixture of tetrasodlum
pyrophosphate and sodlum acid pyrophosphate, the same problems
occurred, but less severely. The addltlon of the inorganic
pyrophosphates in dry form to the dry ingredients in the dough
preparation basically eliminated the above problems. It was
also found that better results were secured by using the
lnorganlc phosphates in powder form as opposed to granular
form.
The lnorganlc pyrophosphates are preferably alkali
metal pyrophosphates. The preferred alkali metal pyrophos-
phates are tetrasodlum pyrophosphate and tetrapotasslum pyro-
phosphate. An example of a useful tetraalkall metal pyrophos-
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1338173
phate ls tetrallthlum pyrophosphate. Alkallne earth metal
pyrophosphates are also useful, but they are generally lnsol-
uble ln water. Preferably, the lnorganlc pyrophosphates are
soluble ln water.
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1338179
Examples of dialkaline metal pyrophosphates are dicalcium
pyrophosphate, dibarium pyrophosphate and dimagnesium
pyrophosphate. Trialkali metal monoacid pyrophosphates, such as,
trisodium hydrogen pyrophosphate, can be used. Monoalkali metal
triacid pyrophosphates, such as, disodium trihydrogen
pyrophosphate, can also be present in limited amounts. Examples
of other inorganic pyrophosphates include manganese pyrophosphate
and dizinc pyrophosphate.
Tetrasodium pyrophosphate, one part, is soluble in 13 parts
of cold water and in 2.5 parts of boiling water. It is insoluble
in ethanol. Dicalcium pyrophosphate is practically insoluble in
water. The invention use of the term "solution" includes
solutions, slurries, suspensions and the like. Tetrapotassium
pyrophosphate is freely soluble in water and is insoluble in
ethanol.
Most preferably a mixture of sodium acid pyrophosphate and
tetrapotassium pyrophosphate is used (in a ratio to achieve the
desired pH).
The maximum allowable GRAS level in a composition for sodium
acid pyrophosphate (SAPP) is 2.1 weight percent and tetrapotassium
pyrophosphate (TKPP) is 1.4 weight percent in baked goods. If
~RAS levels change (rise) or if higher levels are allowed by the
regulatory agencies, higher levels can be used in the invention.
TKPP delivers approximately 52.65 percent of P207; SAPP delivers
about 78.36 percent of P207; and TSPP delivers about 65.4 percent
of P207-
The most preferred invention dough contains trisodiummonoacid pyrophosphate (that is, sodium acid pyrophosphate or
133817~
SAPP) and tetrapotassium pyrophosphate in a weight ratio of about
60 to 40.
The pyrophosphate(s) is used in sufficient amount to deliver
generally from about 0.1 to about 5, preferably from about 0.5 to
about 3.5, most preferably 1.4 to 2.5 weight percent (based on the
total composition), of P2O7.
A study of the application of aqueous solutions of a mixture
of tetrasodium pyrophosphate and sodium acid pyrophosphate to the
teeth of dogs by spraying for one month resulted in dose response
data. The aqueous solutions containing S and 3 weight percent of
a mixture tetrasodium pyrophosphate and sodium acid pyrophosphate
resulted in significant reductions in tartar accumulation. The
aqueous solutions containing 1.5 and 0.5 weight percent of a
mixture of sodium acid pyrophosphate and tetrasodium pyrophosphate
resulted in directional trends of reductions in tartar
accumulation. See also U.S. Patent No. 3,323,551.
The ratio of sodium acid pyrophosphate (SAPP) to
tetrapotassium pyrophosphate (TKPP) is generally between 4 to 1
and 3 to 7, preferably between 7 to 3 and 1 to 1, most preferably
about 3 to about 2. SAPP has a pH of 4.2 and TKPP (and TSPP) has
a pH of 10.2, so the combination of SAPP and TKPP (or TSPP)
provides a resultant pH which is a balance of the pHs of the two
components.
The pH of the dough of the inner portion containing at least
one inorganic pyrophosphate compound (salt) is generally in the
range of about 4 to about 10.5, typically from about 4.5 to about
7.5, preferably from about 5 to about 7, most preferably between
about 5.6 dog biscuit has a pH of 6.1 and about 6.1. Milk Bone~
88
- 1338179
dog biscuit has a pH of 6.1 to 6.4. Tartar reduction is indicated
to be best at a neutral pH and palatability is indicated to be
best at a slightly acidic pH, so the best mode contemplates a
balance of such two factors in any commercial product.
The coating solution application is usually conducted at a
temperature of about 45 to about 140F, preferably about 60 to
about 12SF.
The dog biscuit dough for the outer portion and the inner
portion can be mixed using any suitable or conventional equipment.
For example, the mixing can be at 20 to 100 rpm. For example, a
dry blending step (dries and the inorganic pyrophosphates) can be
done typically at room temperature for a period of time of about 3
minutes to about 20 minutes. The dry-blended mixture can then be
mixed with the hot water to form a first stage dough. The water
which can be admixed with the dry-blended mixture is typically at
a temperature of about 65 to about 150F. The hot water can be
added, with mixing, over a period of time of about 3 minutes to
about 6 minutes to form the first stage dough. Then, the fat
portion of the biscuit dough can be admixed with the first stage
dough to form the final stage dough. The fat portion can be added
at a temperature at which it is at least fluid, typically at about
100 to about 150F. The fat portion can be mixed for a period of
time which is sufficient to form a dough whose homogeneity is
visually apparent. A typically final mixing time is about 3 to
about S minutes.
If there are machinability and dough structure property
problems with the center portion dough, the addition of water
should solve such problems. If the use of the higher water levels
89
1~817~
caused the dough to be so sticky as to cause problems in a sigma
or rotary mixer (but normally not a significant problem in a
continuous mixer). The addition of more tallow to the dog biscuit
dough should assist in more effective mixing and help to keep the
dough from being so sticky that it clings to a rotary molder.
Preferably the tallow level is about 2.6 to about 3.1 weight
percent (most preferably about 2.85 weight percent), as opposed to
a tallow level of about 5 dog biscuits. Also, 2.46 weight percent
in Milk Bon ~ the tallow provides a taste which dogs like.
Formation of the dough is achieved at about atmospheric
pressure with mixing of the components being conveniently achieved
in an upright sigma blade mixer or other bakery-type mixers. The
various ingredients can be added over a period of time or in a
one-shot manner according to the above order of addition.
However, melted fat and water can be added simultaneously and
mixed for 6 to 10 minutes.
The center portion of the dog biscuit can also be a fruit
filler, e.g., a fruit gel composition, containing at least one
inorganic pyrophosphate.
The dog food composition, such as, dog biscuits, having a
soft center portion can be prepared by any suitable method, such
~s, convention deposition of the center portion on a dough piece
and then capped by another dough piece, the edges of such pieces
preferably being pressed together. Such dough pieces can be
formed in any suitable or conventional manner, such as, by
extrusion, stamping, cutting or molding. Preferably the food
composition is prepared by the coextrusion of the outer portion
and the soft center portion. Any suitable dog food composition
1338l7~
shapes or dog biscuit shapes can be used, such as, bone-shaped
canine biscuits. Holes can be formed in the dog food composition
or dog biscuits to facilitate the escape of moisture during
baking, cooking and/or drying.
The dog biscuit dough pieces can be baked using any suitable
or conventional equipment and conditions. For example, the dog
biscuit dough pieces can be passed into an oven such as a
conventional band oven where the biscuits are baked. The conveyor
belts of the oven can be coated with an edible lubricant such as a
natural or synthetic cooking oil or shortening to facilitate
separation from the conveyor belts of the baked products.
Temperatures in the range of about 300 to about 600F can be
used. The baked dog biscuits can also be subjected to subsequent
drying at temperatures of about 200 to 400F, either within the
baking oven or separately, to produce the desired moisture content
in the final product.
The formed dog biscuit dough pieces are baked, followed by
drying, to achieve a shelf stable product without the need of any
moisture barrier protection. Baking and drying temperatures and
times are those conventionally used in the production of a dry
canine biscuit. The pieces are dried to obta~n a biscuit having a
water activity of 0.70 or less. Typically, baking temperatures
and times are about 300F to about an average of 475 for about 25
minutes to about 8 minutes. Drying conditions are typically about
200 to - about 325F for about 25 minutes to about 12 minutes in
a forced air dryer. On a weight basis, the moisture content of
the final biscuit product is less than or equal to about 15
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1338179
percent by weight and preferably about 10 to 12 percent by
weight of the flnal biscult at 70 percent relative humldity.
The invention product does not lnclude any fluorine-
containing compound or other fluoride lon source, or
quaternary ammonium compounds. Also the invention product
does not include any organic pyrophosphates.
The invention deals primarily with dogs, but has a
scope of teeth-bearing non-human, mammals, such as, cats.
The invention composition can be used to reduce and
control tartar accumulation on canine teeth. Based upon dog
biscuits 12 the weight of commercial Milk ~one~ small inven-
tion dog biscuits per day, 10 medium invention dog biscuits
per day, 6 large invention dog biscuits per day or 4 extra
large invention dog biscuits per day will supply about 1/4 to
1/3 of a dog's caloric requirement.
The invention also involves anlmal foods, such as,
dog foods, having a coating containing at least one inorganic
pyrophosphate. The above lnformation regarding inorganic
pyrophosphates also applies here; the coating can contain the
same amounts and type of lnorganic pyrophosphates as in the
case of the soft center portion.
The coating is preferably applied to the animal food
in the form of a llquefied coatlng formulatlon by any sultable
means, such as, dipping, spraying, etc. The coatlng can
encompass all or part of the anlmal food.
The liquefied coatlng formulatlon best contalns at
least one suspension agent. The preferred suspenslon agent is
a polysaccharide gum, most preferably xanthan gum. Preferably
about
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0.05 to 1.75 weight percent of polysaccharide gum (xanthan gum) is
used. Xanthan gum is one of the few gums which acts as an
acceptable suspension agent in the invention. The xanthan gum is
an excellent agent for controlling the bodying effect, as it is
stable over a broad temperature range, i.e., it holds the same
viscosity over a large temperature range without any separation of
the coating ingredients. The xanthan gum has a bodying effect so
that little or no separation occurs. Other suitable gums and
mucilages can be used.
Malto-dextrin produced by hydrolyzing corn starch is
preferred; it serves as a carrier (bodying), binding agent and
suspension agent and helps the appearance of the coating; and it
is a preferred ingredient. Other malto-dextrins can also be used
for the same functions.
An adhesive or binding agent,-such as, malto-dextrins, is
needed in the coating slurry, to help the coating material bind
(adhere) to the raw hide when the raw hide is dipped in the
coating slurry. Preferably about 5 to about 15 weight percent of
the malto-dextrin is included in the coating material.
A carrier, such as, starch or a modified food starch, is
included in the coating formulation. Preferably about O.1 to
~about 5 weight percent of the food starch or modified food starch
is included in the coating material. The food starch or modified
food starch also serves to control the viscosity.
Animal fat preferably is included for flavor purposes. Other
suitable flavorants can be used or included, particularly salt.
The flavorants can be any dairy product flavorant, such as milk or
93
1~817~
cheese, meat flavorants, such as, liver or beef, poultry and fish.
Flavorants help provide palatability for the invention coating.
Preferably a hydrogenated vegetable oil is included in the
coating formulation for sheen and to modify the melting point of
the formula fats in the finished product. It also helps to
prevent flaking of the coating; also the coating does not have a
tacky feeling.
Any suitable colorant can be included in the coating
formulation. The preferred colorant is caramel color which also
provides some flavor to the product.
The coating also incorporates sufficient water to achieve the
liquefied coating composition. Amounts of the other ingredients
are those which are effective to achieve their functions in the
coating formulation.
The preferred coating formulation, besides the inorganic
pyrophosphates, contain animal fat, a surfactant, such as, a
modified lethicin, polysaccharide gum, a modified food starch,
flavorant, colorant, hydrogenated vegetable oil, a carrier, such
as a malto-dextrin, and water. A suitable humectant, preferably
propylene glycol, can be used in the coating formulation.
The coating formulation should be viscous enough so that the
coating formulation generally only coats the surface regions of
the animal food. The presence of coating in the surface regions
of the animal food helps to anchor the resultant coating and to
prevent the coating from easily being separated from the animal
food during handling and shipping. Basically though the coating
is strictly a surface phenomena on the animal food.
The coating slurry can be applied to the animal food by any
suitable means, such as, spraying, dipping, soaking in a
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container, etc. The coating slurry is applied generally at a
temperature of 45 to 200F, preferably at about 60 to about
190F, and most preferably at about 180F. The coating slurry has
a low microbial profile at such higher temperatures.
After treating the raw hide with the pyrophosphate slurry,
the coated animal food is dried and/or baked. While the coated
animal food is preferably air dried, it is also advantageous to
dry the coated animal food using applied heat, e.g., in a hot air
oven (at a temperature of say 75F to 300F).
The preferred embodiment and ranges of the above type of
coating is:
Ingredients Percentages
Specific Ranges
Sodium acid pyrophosphate (SAPP),
anhydrous powder, (non-leavening type) 1.73 0.25 to 5
Tetrapotassium pyrophosphate
(TKPP), anhydrous powder 1.15 0.25 to 5
Salt 0.50 0.05 to 2.5
Malto-Dextrin 9.17 2 to 30
Modified Food Starch 2.00 0.1 to 10
Colorant 0.50 0.01 to 3
Flavorant 2.00 , 0.01 to 5
Xanthan 0.20 0.05 to 1.5
Lecithin or Modified Lecithin 1.25 0.5 to 1.75
Vegetable Fat 0.50 0.1 to 3
Animal Fat l_ 0.1 to 5
Subtotal 20.00
Water 80.00 50 to 97
Total 100.00
133817~
The following coating-baking procedure is particularly
advantageous:
(a) dry blending the dry powder.
(b) adding 1/4 of the water and slurring the composition.
(c) adding remaining 3/4 of the water and mixing to form
the coating formulation.
(d) heating the coating formulation to 185 to 200F with
intermittent stirring (add animal fat at about 125F
during the heating).
(e) maintaining the coating formulation at 160 to 190F.
(f) apply the coating material to the unbaked dough pieces.
(g) baking the coated, unbaked dough pieces at 325F for 25
minutes.
(h) drying the baked, coated dough pieces for 25 minutes at
225F in a forced-air dryer.
The animal food within the scope of this invention needs to
have a sufficient integrity to not fall apart during processing
and handling, especially, so that the coating can be applied,
dried/baked, etc., without losing its integrity or cracking. The
animal food is best in the form of pieces or the like, such as,
kibbles, biscuits, snacks, etc. The animal food pieces can be
made by any suitable forming means, such as, extruding, molding,
stamping, etc. The invention composition is used to reduce and
control tartar accumulation on canine teeth.
The coating containing at least one inorganic pyrophosphate
salt can be applied to animal foods having soft centers which may
or may not contain at least one inorganic pyrophosphate. The
96
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total amount of inorganic pyrophosphate can be distributed
between the coating and the soft center.
The coating can also be composed of SEALGUM* and at
least one lnorganic pyrophosphate. SEALGUM* ls a tradename of
Colloides Naturals Inc. of Bridgewater, New Jersey 08807 for a
coating material which provides a gummed, shiny coatlng. The
coatlng, for example, can be applied in the form of a sol-
ution, slurry or emulslon by using a rotative coatlng machine
or using spray nozzles.
The animal food can be the dog food dlsclosed ln
commonly-owned U.S. Patent No. 4,904,494, filed on September
9, 1988, entltled "Chewy Dog Snacks", or commonly-owned
copending Canadian Application Serlal No. 610,692, filed on
September 8, 1989, of the same title. A chewy, semi-plastic,
non-extruded, non-porous, microbiologically-stable dog food
whlch lncludes: 12 to about 30 weight percent, based upon the
total weight of the dog food, of gelatin; at least one
acldulant; at least one cereal starch-contalnlng textural
agent; at least one release agent; at least one taste agent;
at least one sugar; salt; and added water. The dog food ls ln
a molded form. The dog food has a pH of about 3 to 5, and has
a molsture content of about 10 to 25 welght percent, based
upon the weight of the dog food. The process for preparlng
the dog food lncludes ~a) mixing the dry components and llquld
components wlth low speed agltatlon and contlnuing the mlxlng
untll a dough ls obtalned; (b) formlng the dough by moldlng
rotary moldlng, etc., lnto molded snacks or blscults; (c)
condltloning the molded (formed) dough at 185 to 200F for
*Trade mark - 97 -
73783-60
13~8179
about 7 to 8 minutes; and (d) packaglng the molded (formed),
baked dog snacks or biscults ln a protectlve package.
The coatlng and dog blscults can be those of U.S.
Patent No. 4,822,626, and copendlng commonly-owned Canadlan
Serlal No. 614,325. The blscults with a baked-on proteln-
aceous coatlng, are produced comprlslng steps of
(a) preparlng a dough plece from a dough comprlslng
flour, meal, fat and water;
(b) enroblng the dough plece wlth a vlscous coatlng
formulatlon comprlslng 10 to 30 welght percent
of a dextrln carrler, 10 to 50 welght percent of
meat, 10 to 30 welght percent of a glazlng
agent, 1 to 5 welght percent of polysaccharlde
gum, 5 to 15 welght percent of monosaccharlde
sugar, 5 to 15 welght percent of a dlsaccharlde
sugar, and water, all based upon total dry
sollds; and
(c) baklng the dough plece to form a dry blscult
wlth a baked-on coatlng. The glazlng agent can
comprlse a gelatln or a modlfled food starch,
and the polysaccharlde gum can be a xanthan gum.
The coatlngs are modlfled by the lncluslon of at least one
lnorganlc pyrophosphate.
The lnventlon also lnvolves swab, gauze and other
llke materlals havlng adsorbed/adsorbed thereon a (aqueous)
solutlon containlng at least one inorganic pyrophosphate. The
above lnformatlon regardlng amounts, types, preferred, etc.,
of the lnorganlc pyrophosphates also apply here. The dlsclos-
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ure hereln concernlng pyrophosphate solutlons (aqueous,
water/ethanol, ethanol, etc.~ ls appllcable here. The sol-
utlon preferably contalns a thlckener, preferably a humectant,
such as, corn syrup, sugar and polyalcohols, such as,
propylene glycol (preferred), sorbltol and glycerln.
Swabs are small stlcks havlng a wad of an absorbent
materlal, preferably cotton, usually wound around one end
thereof. Gauze ls a loosely woven cotton (or other sultable
absorbent materlal) surglcal dresslng. The gauze can have a
water-proof backing.
The solution (preferably aqueous) contalnlng
pyrophosphate can be applled to the swab, gauze and llke
materlals by any sultable means. Preferably the sorbent or
tlp portlon of the swabs contalnlng the cotton or llke
materlal ls dlpped into the solutlon whlch ls usually heated
at 45 to 200F, preferably at about 60 to about 190F, and
most preferably at about 180F. The treated swab can be
packaged ln a llquld-tlght contalner wlthout drylng. The
treated swab can also be drled, preferably ln a forced-alr
oven at a temperature of 75 to 300F. The gauze ls preferab-
ly dlpped ln the solutlon or sprayed wlth the solutlon. The
solutlons are usually and preferably heated as above. The
treated gauze can be packaged ln a llquid-tlght contalner or
packaged wlthout drylng. The treated gauze can also be drled
as above.
The undrled or drled swabs, gauze or like material
are packaged, indivldually or ln plurallty, ln llquld-tlght or
alr-tlght contalners.
_ 99 _
D 73783-60
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The undrled or drled swabs, gauze or llke materlal
can be used to control or reduce tartar accumulatlon on anlmal
teeth, such as, dog teeth, by contactlng such teeth on a
perlodlc basls
- 99a -
D 73783-60
1338179
(preferably each day) with such dried, coated swabs, gauze or like
material.
The invention further involves swabs, gauze and other like
materials having thereon and/or therein a coating containing at
least one inorganic pyrophosphate. The above information
regarding amounts, types, preferred, etc., inorganic
pyrophosphates also applies here. The coating can contain the
same amounts and type of inorganic pyrophosphates as in the case
of the soft center portion.
The coating preferably is the coating described above which
contains a surfactant, such as, lecithin or modified lecithin,
xanthan gum (or other suitable polysaccharide gum), a starch or
modified food starch, hydrogenated vegetable oil and a carrier,
such as, malto-dextrin, flavorant (optional) and colorant
(optional), but not including the animal fat. The above
disclosure regarding such coating also applies to this invention
embodiment, as appropriate. A suitable humectant, preferably
propylene glycol, can be used in the coating formulation.
The coating can be applied to the swab, gauze and like
materials by any suitable means. Preferably the sorbent or tip
portion of the swabs containing the cotton or like material is
~dipped into the liquefied coating composition, which is usually
heated at 45 to 200F, preferably at about 60 to about 190F,
and most preferably at about 180F. The coating can then be dried,
preferably in a forced-air oven at a temperature of 75 to 300F.
The gauze is preferably dipped in the liquefied coating
composition or sprayed with the liquefied coating composition.
100
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The llquefled coating composltlons are usually and preferably
heated as above and the drying is preferably done as above.
The dried, coated swabs, gauze or llke materlal are
packaged lndlvldually or ln plurality, in alr-tlght con-
tainers.
The dried, coated swabs, gauze or llke material can
be used to control or reduce tartar accumulation on anlmal
teeth, such as, dog teeth, by contactlng such teeth on a
periodlc basls (preferably each day) wlth such drled, coated
swabs, gauze or like materlal.
The lnvention involves meat ~erky, such as, beef
~erky, havlng adsorbed/adsorbed thereln and/or thereon a
(drled or undrled) solutlon contalnlng a (aqueous) solutlon
contalnlng at least one lnorganlc pyrophosphate. The above
lnformatlon regardlng amounts, types, preferred, etc., of the
lnorganlc pyrophosphates also applles here. The solution
should use an aqueous, water/ethanol or ethanol solvent. As
used ln thls entlre document, a solutlon can lnclude a slurry,
suspension or the llke where approprlate, for example, lf a
water-lnsoluble pyrophosphate ls used.
The solution can be applied to the meat ~erky by any
sultable means. The meat ~erky, partlcularly beef ~erky, ls
somewhat porous in structure. The solution is preferably
applied by dlpplng the meat ~erky ln the solutlon, whlch ls
usually at 45 to 200F, preferably at about 60 to about
l90~F and most preferably at about 180F, or by spraylng the
solutlon onto the meat ~erky (the solutlon temperatures belng
the same as above). The treated meat ~erky can be drled by
- 101 -
D 73783-60
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any sultable means, preferably ln a forced-alr oven at a
temperature of 75 to 300F.
- lOla -
D 73783-60
1~38179 73783-60
The meat jerky can be packaged in air-tight containers.
Any meat jerky can be used. Naturally prepared jerky,
also known as charqui, typically made with strips of striate
muscle meat. Beef jerky products for canine consumption are
usually prepared by the loaf extrusion method, the single strip
extrusion method and the ribbon strip extrusion method.
Coextensively aligned jerky are described in Canadian Patent No.
1,298,139 and copending, commonly-owned Canadian Application
Serial No. 560,935.
The meat jerky can be used to prevent or reduce tartar
accumulation on animal teeth, such as, dog teeth, by having the
animal consume the treated meat jerky on a periodical (e.g.,
daily) basis.
The invention involves meat jerky, such as, beef jerky,
having thereon and/or therein a coating containing at least one
inorganic pyrophosphate. The above information regarding the
amounts, types, preferred, etc., of inorganic pyrophosphates
applies here.
The coating preferably is the coating described above
which contains a surfactant, such as, lecithin or modified
lecithin, xanthan gum (or other suitable polysaccharide gum), a
starch or modified food starch, hydrogenated vegetable oil, a
carrier, such as, malto-dextrin, animal fat, flavorant, colorant
and water. The above disclosure regarding such coating also
applied to this invention embodiment, as appropriate. A suitable
humectant, preferably propylene glycol, can be used in the coating
formulation.
A 102
1338l7g
The coating can be applied to the meat jerky gauze and like
materials by any suitable means. Preferably the meat jerky is
dipped into or sprayed with the liquefied coating composition,
which is usually heated at 45 to 200F, preferably at about 60
to about 190F, and most preferably at about 180F. The coating
can then be dried, preferably in a forced-air oven at a
temperature of 75 to 300F.
The dried, coated meat jerky is packaged in air-tight
containers.
The dried, coated, meat jerky can be used to reduce or reduce
tartar accumulation on animal teeth, such as, dog teeth, by having
the animal consume the treated meat jerky on a periodical (e.g.,
daily) basis.
The invention also includes the application of a solution
containing at least one inorganic pyrophosphate onto an animal
food, such as, dog biscuits, semi-moist dog food, kibbles,
extruded dog snacks and food, coated dog biscuits, etc. The above
information regarding amounts, types, etc., of the inorganic
pyrophosphate also applies here. Preferably the edible solvent
used in the solution is water.
The solution is preferably applied to the animal food by
~means of a spray device, e.g., a spray bottle or a spray can. The
treated animal food is used to reduce or prevent tartar
accumulation on the animal's teeth, for example, dog teeth or cat
teeth, by having the animal consume such treated animal food on a
periodic (e.g., daily) basis.
The following is a summary of experiments described in more
detail below:
103
1338179
Definitions:
SAPP is sodium acid pyrophosphate (or trisodium monoacid
pyrophosphate or sodium pyrophosphate).
TSPP is tetrasodium pyrophosphate.
TKPP is tetrapotassium pyrophosphate.
xample 1: Initial testing of solutions of pyrophosphates.
Solutions were applied directly to teeth.
xample 2: Addition of pyrophosphate (5 percent delivered) to
Milk Bone~ formula. Milk Bon ~ is a registered
trademark of Nabisco Brands, Inc. for canine
biscuits.
xamPle 3: Dose response study. Pyrophosphate at 0.5, 1.5,
3.0 and 5.0 percent delivered were added to the
Milk Bon ~ formula.
Examples 2 and 3 are based upon modifications of the formula
of Milk Bone dog biscuits.
104
1338l79
Table 4
TARTAR CONTROL BISCUITS
SUMMARY OF FORMULA DEVELOPMENT
Control Ex. 2 Ex. 3
Regular 5~ Pyro- Dose
Milk Bone~ Phosphate Study,
Ingredients Lbs. Lbs. Lbs.
Flour 940.000 940.000 See
Soybean Meal 135.000 135.000
Meat & Bone Meal100.000 100.000 Example
Wheat Meal 40.000 40.000
Tallow 32.000 32.000 3
Salt 10.000 10.000
Dicalcium Phosphate8.500 8.500
Natural Flavorants17.000 17.000
Bone Meal 5.000 5.000
Calcium Carbonate 2.000 2.000
Dough Conditioners2.875 2.875
Vitamin Premix 0.375 0.375
Tetrasodium Pyrophosphate -0- 70.280
Sodium Acid Pyrophosphate -O- 23.450
Tetrapotassium
Pyrophosphate -o- -~-
`Calcium -0- -0-
TOTAL1,292.7501,386.48
105
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Example 1
Solution Tests
Purpose
To determine the dose response of three concentrations of
an anti-tartar agent (pyrophosphate) to reduce accumulation of
tartar formation in the dog.
Test Design
Treatment
DI H2O - Control
3.3% Pyrophosphate
5.0% Pyrophosphate
6.7% Pyrophosphate
Test Solutions
Formulas
Tetrasodium Sodium Acid % Delivered
Pyrophosphate (TSPP) Pyrophosphate (SAPP) Pyrophosphate
3.58 grams 1.22 grams 3.3
5.42 grams 1.85 grams 5.0
7.27 grams 2.48 grams 6.7
The above pyrophosphates were mixed with 100 ml of DI H20. The
test solutions were applied to the teeth using a modified
syringe. The ratio of the above blends of TSPP and SAPP is:
TSPP-75 percent, SAPP-25 percent.
pH of Test Solutions
Test Solutions ~
3.3% 7.92
5.0% 7.74
6.7% 7.85
Results
A significant reduction in tartar accumulation was shown
with the 5 percent pyrophosphate solution.
106
133~179
Example 2
Pilot Plant Study With Milk Bon P
Containing 5 Percent of Deliverable Pyrophosphate
Purpose
The addition of pyrophosphate to Milk Bon ~ dog biscuits.
Test
Tetrasodium pyrophosphate (TSPP) and sodium acid
pyrophosphate (SAPP) were used. The ratio of the
pyrophosphates was 75 percent of TSPP and 25 percent of SAPP.
The level of TSPP was 5.1 percent and SAPP was 1.69 percent of
the formula weight--which delivers approximately 5.0 percent
of pyrophosphate. The TSPP and SAPP, dissolved in water, were
just added to the total weight of the regular Milk Bon ~
formula. No other formula adjustments were made so that the
effects of the pyrophosphates could be determined.
The study originally was designed to test Milk Bon ~ with
5.0, 7.5 and 10.0 percent of deliverable pyrophosphate. At
the 7.5 and 10.0 percent levels, acceptable biscuits could not
be rotary molded. The finished product was extremely soft and
had distorted shapes. Biscuits with 5.0 percent of
pyrophosphate were borderline acceptable. The color of the
biscuits were whitish in color, whereas the control biscuits
are tan/beige in color.
Results
A significant reduction in the accumulation of tartar was
seen at the 5 percent pyrophosphate level. There was a
significant amount of breakage (30 to 35 percent) with the 5
percent pyrophosphate biscuits.
107
133817~
Additional Information
pH of biscuits:
Control Milk Bone~ - 6.15
5 percent of pyrophosphate Milk Bone~ - 6.98
Example 3
Pilot Plant Dose Response Study
Purpose
To establish a dose level which is effective for tartar
control.
Test
The TSPP and SAPP solutions were added to the weight of
the regular Milk Bone~ formula. No other formula adjustments
were made so that the effect of the pyrophosphates could be
determined. The pyrophosphates were dissolved in water (135
to 140F) and added to the Milk Bon ~ dries. Regular medium
Milk Bone~ and four medium Milk Bone~ test products were made.
Each of the test products contained different levels, 0.5,
1.5, 3.0 and 5.0 percent of deliverable pyrophosphates. The
ratio of the blend of tetrasodium pyrophosphate (TSPP) and
sodium acid pyrophosphate (SAPP) was:
TSPP - 75%}
~ for all four levels
SAPP - 25~}
The total amounts of TSPP and SAPP added to the formula and
approximate delivered soluble pyrophosphate (P2O7) were:
108
133817!~
% % % %
(75%) TSPP added -0.54 1.603.17 5.10
(25%) SAPP added -0.18 0.531.10 1.69
Total 0.72 2.134.27 6.79
Approx. delivery
of soluble pyro-
phosphate - 0.5% 1.5%3.0% 5.0%
Pilot Plant Trials
The doughs containing 0.5 and 1.5 percent of delivered
pyrophosphates were similar in development to control regular
Milk Bon ~ dog biscuits. However, the doughs with the 3 and 5
percent levels were shorter in texture and not as developed as
the control. The finished products at these two levels were
less hard than the control biscuits.
~H - of Biscuits (10% solution)
Regular Milk Bon ~ - 6.10
0.5% biscuits - 6.41
1.5% biscuits - 6.75
3.0% biscuits - 6.88
5.0% biscuits - 7.07
Results of the Study
Pyrophosphate
Delivery Results
0.5% Milk Bon ~ biscuits No significant reduction in
tartar accumulation -
directional trend
1.5% Milk Bon ~ biscuits No significant reduction in
tartar accumulation -
directional trend
3.0% Milk Bone~ biscuits A significant reduction in
tartar accumulation
109
1338179
.0% Milk Bon ~ biscuits A significant reduction in
tartar accumulation
A significant amount of breakage (approx. 25 percent) was
reported for the 5 percent pyrophosphate biscuits. There was
approximately 15 percent breakage with the 3 percent level.
At the 0.5 and 1.5 percent of pyrophosphate levels, the
breakage was not considered excessive compared to the control
biscuits.
Test data and results are set out in the following table:
110
- 1338179
TABLE 5
REGULAR MILK BONER/PTKOR; - IIATE/TARTAR CONTROL
DOSE RESPONSE STUDY
PYRO- PYRO-
CONTINUOUS PHOSPHATE PHOSPHATE
MIX CONTROL .50X 1.50%
INGREDIENTS LBS PERCENT LBS. PERCENTLbs. PERCENT
Flour 940.00 72.7132 940.00 72.1855940.00 71.1604
Soy Heal 135.00 10.4429 135.0010.3671 135.00 10.2198
Meat ~ Bone Meal 100.00 7.n54 100.00 7.6793100.00 7.5703
~heat Meal 40.00 3.0942 40.00 3.071740.00 3.0281
Tallo~ 32.00 2.4753 32.00 2.457432.00 2.4225
Salt 10.00 o. m 5 10.00 0.767910.00 0.7570
Dicalcium Phosphate 8.50 0.6575 8.50 0.65278.50 0.6435
Natural Flavorants 17.00 1.3157 17.00 1.305617.00 1.2869
Bone Meal 5.00 0.3868 5.00 0.38405.00 0.3785
Calcium Carbonate 2.00 0.1547 2.00 0.15362.00 0.1514
Dough Conditioners 2.875 0.2224 2.875 0.22082.875 0.2176
Vitamin Premix 0.375 0.0290 0.375 0.02880.375 0.0284
Tetrasodium Py.u~,uD~hate -0- -0- 7.07 0.5429 21.14 1.6003
Sodium Acid Py,u~h~a~.ate -0- -0- 2.38 0.1828 7.07 0.5352
TOTAL 1,292.75 1,302.2 1,320.96
111
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TABLE 5 (CONT.)
PrRO- PrRO-
PHOSPHATE PHOSPHATE
3.0% 5.0%
INGREDIENTS LBS. PERCENT BS. PERCENT
Flour 940.00 69.6797 940.00 67.7976
Soy Meal 135.00 10.0072 135.00 9.7369
Meat & Bone Meal 100.00 7.4127 100.00 7.2125
~heat Meal 40.00 2.9651 40.00 2.8850
Tallo~ 32.00 2.3721 32.00 2.3080
Salt 10.00 0.7413 10.00 0.7213
Dicalcium Phosphate 8.50 0.6301 8.50 0.6131
Natural Flavorants 17.00 1.2601 17.00 1.2261
Bone Meal 5.00 0.3706 5.00 0.3606
Calcium Carbonate 2.00 0.1483 2.00 0.1443
Dough Conditioners 2.875 0.2132 2.875 0.2074
Vitamin Premix 0.375 0.0278 0.375 0.0270
Tetrasodium Py,u~ho~,ate 42.210 3.1289 70.28 5.0689
Sodium Acid Py~u~,o~,ate 14.070 1.0430 23.45 1.6913
TOTAL 1,349.03 1,386.48
112
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The following is a summary of experiments described in
more detail below:
xample 4: Initial testing of solutions of pyrophosphates.
Solutions were applied directly to teeth. Same
as Example 1.
xample 5: Addition of pyrophosphate (5 percent delivered)
to Milk Bon ~ formula. Same as Example 2.
xample 6: Dose response study. Pyrophosphate at 0.5,
1.5, 3.0 and 5.0 percent delivered were added
to the Milk Bon ~ formula. Same as Example 3.
xamPle 7: Base line formula. Used to determine the
effects of pyrophosphate on the nutritional
aspects of Milk Bon ~ formula.
xample 8: 2.57 percent pyrophosphate delivery. This
formula was modified to balance calcium and
phosphorus ratio (eliminated dicalcium
phosphate and bone meal, and increased calcium
carbonate).
xample 9: 2.34 percent pyrophosphate delivery. This
formula was modified to balance sodium and
chloride (substituted TKPP for TSPP, eliminated
salt, added CaCl2 and reduced CaC03).
xample 10: Same as Example 9, but with increased tallow
(and increased water).
xample 11: Lower pyrophosphate delivery (1.6 percent
pyrophosphate) than Example 10.
Examples 4 to 11 are based upon modifications of the
ormula of Milk Bon ~ dog biscuits.
113
133817~
TABLE 6
TARTAR CONTROL BISCUITS
SUMMARr OF FORMULA DEVELOPMENT
EX. 8 EX. 9 EX. 10
CONTROL EX. 5 EX. 6 EX. 7 FORMULA FORMULAFORMULA
REGULAR 5% PYRO- DOSE BASELINE#3 2.5Z 4A 2.3%4B 2.34%
MILK BONEPHOSP~ATESTUDYFORMULA PYRO. PYRO. PYRO.
INGREDIENTS LBS. LBS. LBS. LBS. LBS. LBS. LBS.
Flour 940.000940.000 See 940.000 940.000940.000 940.000
Soybean Meal 135.000 135.000 135.000135.000 135.000135.000
Meat & Bone Meal 100.000 100.000Example100.000100.000 100.000100.000
wheat Meal 40.000 40.000 40.000 40.000 40.000 40.000
Tallow 32.000 32.000 No. 3 32.000 32.000 32.000 37.000
Salt 10.000 10.000 10.000
Dicalcium Phosphate8.500 8.500 8.500 -0- -0- -0-
Natural Flavorants17.000 17.000 17.000 17.000 17.000 17.000
Bone Meal 5.000 5.000 5.000 -0- -0- -0-
Calcium Carbonate 2.000 2.000 2.000 37.000 25.000 25.000
Dough Conditioners2.875 2.875 2.875 2.875 2.875 2.875
Vitamin Premix 0.375 0.375 0.375 0.375 0.375 0.375
Tetrasodium PyIo~,os~,ate -0- 70.280 18.800 19.000 -0- -0-
Sodium Acid Pyro~,os~,ate -0- 23.450 28.200 28.500 27.000 27.000
Tetrapotassium Py,u~,os~,ate -0- -0- -0- -0- 18.000 18.000
Calcium Chloride -0- -0- -0- -0- 13.500 13.500
TOTAL 1,292.7501,386.48 1,339.7501,375.2501,350.750 1,355.25
Note: 1. Example 10 rapr~s_,ts a preferred formula having 2.34 ~eight percent of ~t,u~ho~,ate.
11~
1338179
Example 7
- TSPP AND SAPP added at appropriate ratio and
levels
- No other formula changes were made
Purpose
The formula serves as a base line formula to determine
the effects of TSPP and SAPP on the nutritional aspects of the
formula. The nutritional data was generated by a computer
program. It was determined that the FDA generally recognized
as safe (GRAS) status for sodium acid pyrophosphate in baked
goods is a maximum level of 2.1 percent and 1.4 percent for
tetrasodium pyrophosphate, therefore, the levels and ratios of
TSPP and SAPP had to be changed.
Chanqes:
The original ratio of TSPP (75 percent) and SAPP (25
percent) was changed to:
SAPP - 60%
TSPP - 40%
To achieve maximum delivery of pyrophosphates the maximum GRAS
allowed levels are used. At these levels the above ratios are
required. TSPP and SAPP were incorporated into the regular
~ilk Bone~ formula - no other changes were made.
Using the allowed maximum levels (TSPP 1.4 percent and
SAPP 2.1 percent) and the new ratios of 60 percent SAPP and 40
percent TSPP the following nutritional data was generated on a
computer program.
115
Results 1338179
Nutritional data:
Calcium -l.lS9%} 1.0
} to
Phosphorus -1.888%} 1.629 Ratio
Potassium -0.813%
Sodium -1.352%
Chloride -0.504%
The calcium and phosphorus ratio per the National Research
Council (NRC) requirements is 1.1:1.4 to 1. In this base line
formula the ratio is reversed, i.e., phosphorus 1.629 to
calcium 1Ø The sodium was high.
Total amount of TSPP and SAPP added = 3.5%
Soluble pyrophosphate delivery = 2.5%
Example 8
2.57% Soluble Pyrophosphate Delivery
Pilot Plant Study
Purpose
To modify formula to balance calcium and phosphorus
ratio. To evaluate the effect of adding TSPP and SAPP in dry
form to the Milk Bone~ formula. In the prior examples the
~yrophosphates were dissolved in water.
Test
To balance calcium and phosphorus ratio, the following
formula changes were made:
- Eliminated dicalcium phosphate - this decreased the
calcium and phosphorus level.
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- Eliminated bone meal - this decreased the calcium
and phosphorus.
Purpose of above changes was primarily to decrease the
phosphorus content.
However, to compensate for the decreases in calcium from
the above change, the following formula change was made:
- Increased calcium carbonate to increase calcium
level.
- Dicalcium phosphate, bone meal and calcium carbonate
are ingredients in regular Milk Bon ~.
- Evaluate the effect of formula changes (omission of
the dicalcium phosphate and bone meal and increase
calcium carbonate) on mixing rotary molding.
Results: Formula #5
Nutritional Data
Calcium 1.807}
) 1.1 to 1.0 ratio
Phosphorus 1.690
Potassium 0.799
Sodium 1.336
Chloride 0.495
Results
The formula of Example 8 has an acceptable calcium to
phosphorus ratio. (It is best not to go over 1.9 percent of
calcium). The lowering of the sodium level and the raising of
the chloride level, but not over the 0.8 percent level, are
recommended. The above nutritional data represents only the
nutrients most affected by the addition of TSPP and SAPP.
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Pilot Plant Trials (Formula of Example 8)
Purpose
To evaluate the effect on dough development of adding
TSPP and SAPP in dry form (blended with Milk Bon ~ dries).
Granular TSPP and SAPP were used for the trials. To evaluate
the affect of the adjustments made by the omission of
dicalcium phosphate and bone meal and the increase of calcium
carbonate. All of the changes influence the water absorption
properties of the formula. The TSPP and SAPP may also
influence the protein (gluten) development.
Results
The granular TSPP and SAPP did not dissolve and could be
seen throughout the dough and finished product. The doughs
were not fully developed (crumbly) and short. With the
addition of extra water the doughs were becoming sticky - this
would create problems with the rotary molding of biscuits.
pH of biscuits: Control 1, 6.12; Example 6(3) formula,
6.36.
This example disclosed: The tetrasodium pyrophosphate
(TSPP) should be with tetrapotassium pyrophosphate (TKPP).
This change will decrease sodium level - but increase
potassium. The salt should be eliminated from the formula.
This change will decrease the sodium and chloride levels.
Calcium chloride should be added. This will increase the
chloride to an acceptable level. However, this change will
also increase the calcium. Therefore, calcium carbonate will
be decreased to keep the calcium and phosphorus ratio in
balance. It is best not to go over 1 percent of calcium
118
133817~
chloride in the formula. There should be a change from
granular to powdered pyrophosphates.
Example 9
2.34% Soluble Pyrophosphate Delivery
Pilot Plant Study
Purpose
To balance the sodium and chloride levels. To produce a
product for palatability kennel testing.
Formula changes:
Changes in the formula were:
Eliminated salt from formula - decreases sodium and-
chloride.
Replaced TSPP with TKPP - decreases sodium - increases
potassium.
Added calcium chloride - to increase chloride.
Decreased calcium carbonate due to addition of calcium
chloride which increased calcium level.
Changed to powdered pyrophosphates instead of granular
pyrophosphates.
Results
Nutritional data
Calcium % 1.843~ 1.16
) to ratio
Phosphorus % 1.585) 1.0
Potassium % 1.252
Sodium % 0.516
Chloride % 0.662
119
- 1338179
The formula was found to be acceptable (nutritionally
balanced). This includes potassium, sodium and chloride.
Tetrapotassium pyrophosphate delivers less pyrophosphate than
(TSPP) tetrasodium pyrophosphate. This is the reason for the
reduction of soluble pyrophosphate delivery.
Pilot Plant Trials
Purpose
To evaluate the use of powdered TKPP and SAPP. To
evaluate the effect on dough and finished product due to
ingredient changes in formula.
Results
The powdered TKPP and SAPP were not visible (by eye)
throughout the dough and finished product. The development of
the dough was approximately the same as in the formula of
Example 8. It was short and on the crumbly side and
approaching stickiness. It was felt that the addition of more
water would increase stickiness and result in poor machining
of biscuits.
pH of Biscuits; control 6.0; formula of Example 9, 5.75
This example disclosed the following changes should be
made: The addition of more tallow. Standard Milk Bon ~
formula contains 32 pounds of tallow - will increase to 37
pounds. With the addition of extra tallow, extra water will
be added to the formula to help minimize dough stickiness.
The extra tallow should also improve palatability.
Palatability Kennel Test Results - Formula of Example 9.
Kennel Test
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1338179
Control (regular Milk Bone~ formula) vs. Formula of Example 9
(standard water and standard tallow level).
Results - No significant preference was shown between the two
products.
Example 10
2.34% Soluble Pyrophosphate Delivery
Pilot Plant Study
Purpose
To evaluate the mixing, machining and finished product of
the Formula of Example 9 with a slight increase in tallow.
With the addition of extra tallow, the water will be increased
for better dough development.
Formula Changes
Increased tallow from 32 pounds to 37 pounds.
Results
Nutritional Data - Formula of Example 10
See below.
pH of biscuits: control, 6.1; Formula of Example
10, 5.8.
Pilot Plant Trials
Purpose
Same as above.
Three batches were made: (1) control standard Milk Bone~
formula; (2) pyrophosphate biscuits (Test #l) with previous
water level; (3) pyrophosphate biscuits (Test #2) with
increased water. Test #1 and Test #2 - have the same
increased level of tallow. Sufficient quantities of the three
batches were made for palatability kennel testing.
121
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Results
Test #l - used previous water level but lncreased the
tallow. The dough was improved over previous doughs. How-
ever, it stlll was short and crumbly. The finished product
had a rough surface--there was no stickiness.
Test #2 - used increased water and tallow which
resulted in a smoother more developed dough. The flnlshed
product was also smoother with less surface cracks. The
hardness values of the blscults are close to control Mllk
Bone~ hardness.
The tallow and water ad~ustments were made ln the
pilot plant uslng a horlzontal mlxer. The above processlng
lmprovements were evaluated ln actual plant trlals uslng a
continuous mixer with improved processing results.
Kennel Test Results
Kennel Test
Control vs. Test #l - a slgnificant preference was shown for
Test #l product.
Kennel Test:
0 Control vs. Test #2 - a significant preference was shown for
Test #2 product.
This Example ls a preferred composltlon, and Test #2
ls a preferred processlng embodlment.
Nutrltlonal Data - Formula of Example 10
Calclum - 1.843%
Phosphorus - 1.585%
Potasslum - 1.252%
Sodium - 0.516%
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D 73783-60
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Chloride -0.662%
Example 11
1.6% Pyrophosphate Delivery
Pilot Plant Study
Purpose
To develop a Milk Bon ~ formula containing a lower level
of pyrophosphate (SAPP and TKPP). The level is approximately
1.6 percent of delivered pyrophosphate. With the lower levels
of SAPP and TKPP, less formula adjustments are needed to meet
nutritional requirements of the National Research Council
(NRC).
Formula Changes (Example lla)
The changes in this formula are compared to the formula
of Example 10:
Calcium Carbonate - decreased from 37 to 15 lbs.
Calcium Chloride - decreased from 13.5 to 13 lbs.
TKPP - decreased from 18 to 12 lbs.
SAPP - decreased from 27 to 18 lbs.
Sodium Bicarbonate - Added as a leavening agent
Results - Nutritional data
Calcium -1.581%}
~ 1.2 to 1.0 ratio
Phosphorus -1.333%)
Potassium -1.105%
Sodium -0.488%
Chloride -0.651%
The Example lla formula is the most preferred
composition.
123
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Formula - Example llb
This formula is basically the same as the formula of lla.
The only differences are: The meat and bone meal was
decreased from 100 to 90 pounds. The level of the one
component of the natural flavorants (i.e., fish meal) was
increased by 10 pounds.
Results - Nutritional data
Calcium - 1.551%}
} 1.2 to 1.0 ratio
Phosphorus - 1.322%}
Potassium -- 1.099%
Sodium - 0.485%
Chloride - 0.651%
pH of biscuits
Regular Milk Bon ~ - 6.18
Formula Ex. lla - 5.88
Formula Ex. llb - 5.93
Additional Information Regarding the formulas of Examples
lla and llb:
The ratio of the blend of TKPP and SAPP is:
60% of SAPP and 40% of TKPP
The level of each pyrophosphate is:
SAPP - 1.35% of formula total weight
TKPP - 0.899% of formula total weight
Test data and results are set out in the following table:
124
3~3~
TABLE 7
Example 11a
TARTAR COUTROL BISCUITS
PrRu,n NATE - APPROXIMATE DELIVERY 1.6%
INGREDIENTS Lbs. PERCENT
Flour 940.000 70.400
Soy Bean Meal 135.000 10.110
Meat and Bone Meal 100.000 7.489
~heat Feed 40.000 2.996
Tallow 37.000 2.771
Sodium Acid Py,u~,os~,ate Anhydrous 18.000 1.348
tPwd.)
Calcium Carbonate 15.000 1.123
Calcium Chloride ~Pwd.~ Anhydrous13.000 0.974
Tetrapotassium Py,u~,o~,ate Anhydrous
(Pwd.) 12.000 0.899
Natural Flavorants 17.00 1.272
Sodium B'icarbonate 5.000 0.374
Dough Conditioners 2.875 0.216
Vitamin Premix 0.375 0.028
TOTAL 1,335.250 100.000
/~,S
1338:179
TABLE 7 (CONT.)
Example 11b
TARTAR CONTROL 81SCUITS
PrKOF;~ ATE - APPROXIMATE DELIVER~ 1.6X
INGREDIENTS LBS PERCENT
Flour 940.000 70.400
Soy Bean Meal 135.000 10.110
Meat and Bone Meal 90.000 6.740
~heat Feed 40.000 2.996
Tallo~ 37.000 2.771
Sodium Acid Py~o~,os~,ate Anhydrous 18.000 1.348
~Pwd.)
Calcium Carbonate 15.000 1.123
Calcium Chloride (P~d.) Anhydrous 13.000 0.974
Tetrapotassium Pyro~,os~,ate Anhydrous
(Pwd.) 12.000 0.899
Natural Flavorants 5.000 0.374
Sodium Bicarbonate 27.000 2.021
Dough Conditioner 2.875 0.216
Vitamin Premix 0.375 0.028
TOTAL 1,335.250 100.000
EXAMPLES 12 T0 28 1338179
In Examples 12 to 28 the following procedure was used:
The coated raw hide strips were prepared by:
(a) blending the dry powders.
(b) adding 1/4 of the water and slurring the
composition.
(c) adding remaining 3/4 of water and mixing to form the
coating formulation.
(d) heating the coating formulation to 185F to 200F.
with intermittent stirring (add animal fat at about
125F during the heating).
(e) maintaining the coating formulation at 160" to
l90"F,
(f) immersing raw hide strips by dipping in the heated
coating formulation and holding the raw hide strips
to the edge to let drain for aobut 15 seconds.
(g) placing the coated raw hide strips on a screen and
drying at 275F for 7 minutes in a forced-air
laboratory oven.
(h) let the raw hide strips cool and then package them.
Any deviations from such procedure is set out in the specific
examples.
The raw hide strips had a calculated average weight of 17
grams each, although actual weight ranged from 8.5 to 335
grams.
The specific ingredients, conditions, etc., are set out
in the following tables:
127
13~8179
Table 9
Ingredients, Examples
Percentages bY weiqht 12 13 14 15
SAPP
TSPP 2.3 2.3 2.3
Malto-dextrin A 10.0 10.0 5.0
Malto-dextrin B 5.0
Food starch modified 5.0
Colorant 0.5 0.5 0.5 0.5
Flavorant 1.0 1.0 1.0 1.0
Xanthan gum 1.0 1.0 1.0 1.0
Gelatin 6.0
Water 87.5 81.8 81.8 81.8
Heated coating to 180Fyes yes yes yes
pH of mixture at 160F 6.4 5.97 5.87 5.8
Raw hide dry only weight 13.811 24.962 14.705 11.289
24.655 23.957 9.485 17.936
Raw hide wet weight 28.650 21.480 13.399
33.840 27.280 20.420
Dried at 200F for: 15 min. 10 min. 15 min. 10 min.
Raw hide dry weight 25.977 16.738 11.782
27.348 24.825 18.546
- 128 -
73783-60
1338179
Notes 1. The pH of the water was 8Ø
Comments
- In Example 12, the coatlng was thick, had a nlce
appearance and had a weight plck up of 2.7 g.
- In Example 13, the coatlng was very thln, had a
blotchy appearance and dld not adhere evenly on the
raw hide.
- In Example 14, the coatlng was thick and had a nice
appearance.
- In Example 15, the coating was thin and had a blotchy
appearance.
- 129 -
D 73783-60
1338179
Table 10
Ingredients, Examples
Parts by weight 16 17 18
SAPP 3.2 3.2 3.2
TSPP 2.13 2.13 2.13
Malto-dextrin B 10 10 10
Modified Food Starch 2.0 2.0 2.0
Cereal 0.5 0.5 0.5
Flavorant 1.0 1.0 1.0
Xanthan gum 0.2 0.2 0.2
Modified lecithin 1.0
Animal fat 2.0
Water 81.0 80.0 79.0
pH at 160F (coating) 5.9 5.9 5.9
Raw hide dry only weight 18.171 18.843 18.017
14.346 23.897 16.046
Raw hide wet weight 20.340 21.300 20.070
16.730 26.660. 18.020
Dried at 200-225F 15 min. 15 min. 15 min
Raw hide (finished)dry weight 18.613 19.432 18.323
14.553 24.484 16.265
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Notes: 1. The pH of the water was 8.3.
Comments:
- In Example 10, the coating had a blotchy appearance.
- In Example 17, the coating was considered best of
Examples 16 to 18, had an even distribution appearance
and was complete.
- In Example 18, the coating again had a blotchy
appearance.
131
1~3~179
Table 11
Ingredients, Examples
Parts by weight 19 20 21 22 23
SAPP 1.73 1.73 1.73 1.73 1.73
TSPP 1.15 1.15 1.15 1.15 1.15
Malto-dextrin B 11.00 11.00 12.0 11.0 9.67
Modified Food Starch 2.0 2.0 1.5 2.0
Cereal 0.5 0.5 0.5 0.5 0.5
Flavorant 2.42 2.42 2.42 2.42 2.0
Xanthan gum 0.2 0.2 0.2 0.2 0.2
Modified lecithin 1.0 1.0 1.0 1.0 1.0
Animal fat 1.0
Water 80.0 79 80 80 80
Heated coating form. yes yes yes yes yes
to 180F
pH at 160F (coating) 5.9 5.9 6.0 6.0 6.0
Raw hide dry only weight 18.082 16.928 12.983 12.211 15.91715.247 15.037 15.077 15.304 12.073
Raw hide wet weight 21.189 14.690 15.930 15.130 19.160 18.575 18.310 18.000 18.370 14.178
Dried at 225F 15 min. 15 min. 15 min. 15 min. 15 min
Raw hide (finished) 18.846 12,472 13.,621 12.776 16.590
dry weight 15.987 15.688 15.588 15.947 12.586
132
1338173
Notes: 1. The pH of the water was 8.2.
2. Drying at 350 and 325F for 5 minutes curled the raw
hide. It was satisfactory to dry at 300F for 7 minutes.
Comments:
- In Example 19, the coating had a good appearance.
- In Example 20, the coating was better than that of
Example 21 and similar to that of Example 19.
- In Example 21, the coating was satisfactory.
- In Example 22, the coating was similar to those of
Examples 19 and 20 and was better than that of Example
21.
- Example 23, best of all results.
133
133817~
Table 12
Ingredients ExamPles
parts by weight 24 25 26 27 28
SAPP 1.73 1.73 1.73 1.73
TSPP 1.15 1.15 1.15 1.15
Malto-dextrin B 0.5 0.5 0.5 0.5 0.5
Modified Food Starch 9.17 9.5 10.05 8.73 8.81
Colorant 0.5 0.5 0.5 0.5
Flavorant 2.0 2.17 2.0 2.0 2.0
Xanthan gum 0.2 0.2 0.2 0.2 0.2
Modified lecithgran 1.25 1.25 1.25 1.25 1.25
Vegetable fat 0.5 0.5 0.5 0.5 0.5
Animal fat 1.0 1.0 1.0 1.0 1.0
Water 80 80 82.0 79.0 80.0
Heated coating to 180F yes yes yes yes yes
pH at 160F (coating) 5.8-6 5.8 5.7 7.5
Raw hide dry only weight 20.867 32.990 19.134 16.634 12.680 23.233 24.136 13.786 111.883 11.987
Raw hide wet weight 24.140 36.610 22.150 19.040
26.290 27.580 15.900 14.140
Dried at 200-225F 7 min. 7 min. 7 min. 7 min. 7 min.
Raw hide (finished) 21.720 34.056 19.803 17.025
dry weight 23.907 25.015
134
13~8179
otes: 1. The pH of the water was 8.
2. The treated raw hide strips had an average weight of
20.18 g, the untreated raw hide strips had an average
weight of 18.92g, and the average weight pickup was
1.25 g.
Comments:
- In Example 24, the coating was a good one.
- In Example 25, the coating was a good one but had no
color in the formula.
- In Example 26, the coating was a good one.
- In Example 27, the coating formulation had good
dispersion but there was excessive foaming.
- In Example 28, there was less foaming but did not aid
dispersion.
135
